Tag: M.W=300-400

Related Products of 30432-16-7,Some common heterocyclic compound, 30432-16-7, name is 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, molecular formula is C6H8Br4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a two-necked flask, 4-hydroxybenzaldehyde (1) (0.02 mol) and KOH (0.02 mol) were dissolved in absolute ethyl alcohol (100 mL) and the solution was stirred for 30 minutes at room temperature. 1,4-dibromo-2,3-bis(bromomethyl)but-2-ene (2) (0.005 mol) was dissolved in absolute ethanol (25 mL) and added drop-wise to this solution at room temperature with the assistance of a dropping funnel. The mixture was then refluxed and stirred for 10 h. After completion of the reaction, the solution was filtered and the solid matter was obtained. It was washed with deionized water, ethanol and diethyl ether, subsequently. The solid matter was recrystallized using DMF/EtOH (1:1). The synthesized compound was dried with P2O5 in a vacuum oven. Some physical properties, the yield and FT-IR data for compound (3) are given in Table 1 and Table 2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,4-Dibromo-2,3-bis(bromomethyl)but-2-ene, its application will become more common.

Reference:
Article; Uysal, ?aban; Er, Mustafa; Tahtaci, Hakan; Synthetic Communications; vol. 46; 22; (2016); p. 1820 – 1832;,
Bromide – Wikipedia,
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Electric Literature of 6320-40-7, A common heterocyclic compound, 6320-40-7, name is 1,3,5-Tribromo-2-methylbenzene, molecular formula is C7H5Br3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a 100 mL agate ball mill jar, 3.29 g (10 mmol)2,4,6-tribromotoluene, 0.0010 g (0.0010 mmol) 5,10,15,20-tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrin cobalt (II), 6.44 g (50 mmol) 70% t-butyl hydroperoxide aqueous solution and 16.45 g of anhydrous sodium sulfate were mixed uniformly, and the ball mill tank was sealed. At room temperature, the ball milling reaction was performed at a speed of 800 rpm for 16.0 h, and the ball milling was stopped every 1.0 h to release the gas in the ball milling tank. After completion of the reaction, the obtained reaction mixture was dissolved in 30 mL of absolute ethanol and stirred at room temperature for 30.0 min. Filter, wash the obtained filter cake with 2 × 10 mL of absolute ethanol, combine the ethanol solutions, and make the resulting ethanol solution to 100 mL. 20 mL of the obtained solution was removed, desolvated under reduced pressure, and the obtained reaction mixture was separated by column chromatography (V cyclohexane: V ethyl acetate = 4: 1 to 1: 4). The conversion of 2,4,6-tribromotoluene was 31%, and the selectivity of 2,4,6-tribromobenzoic acid was 99%. No other significant oxidation products were detected.

The synthetic route of 6320-40-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Shen Haimin; Qi Bei; She Yuanbin; (18 pag.)CN110563590; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 20027-95-6, name is 1,5-Dibromo-2,6-dimethylnaphthalene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 20027-95-6, category: bromides-buliding-blocks

(1) Synthesis of Intermediate C Intermediate C was synthesized according to the following scheme. In argon atmosphere, 17 g of 1,5-dibromo-2,7-dimethylnaphthalene, 35 g of bispinacolate diboron, 2.8 g of Pd(dppf)Cl2, 22 g of potassium acetate, and 400 ml of DMF were charged into a flask. The mixture was heated under stirring at 80 C for 65 h. After cooling, the precipitate was collected by filtration, washed with water and then toluene, and dried. Then, a mixture of 15 g of the obtained boronic ester, 27 g of bromoiodobenzene, 1.9 g of tetrakis(triphenylphosphine), 26 g of sodium carbonate, 120 ml of water, and 420 ml of DME in a flask was heated under stirring in argon atmosphere at 78 C for 665 h. After cooling, the precipitate was collected by filtration, washed with water and then methanol, and recrystallized from toluene. Then, a mixture of 13 g of the obtained dibrominated compound and 120 ml of pyridine in a flask was heated to 95 C. Thereafter, 10 g of potassium permanganate and 10 ml of ion exchanged water were added to the mixture. Then, 13 portions of 2 g of potassium permanganate and 2 ml of water were added to the mixture every ten minutes. The reaction product solution was hot-filtered and the filtrate was neutralized by a 2 N hydrochloric acid. The precipitated white solids were collected by filtration and washed with water. Finally, a mixture of 15 g of the obtained dicarboxylic compound and 300 ml of a concentrated sulfuric acid in a flask was heated under stirring at 85 C for 3 h. After cooling, the reaction product solution was slowly added to iced water, and the precipitated solids were collected by filtration and washed with ion exchanged water. The solids were further purified by sublimation, to obtain 7 g of the intermediate C. Through IR measurement of the obtained compound, it was found that the absorption attributable to carbonyl group appeared at 1720 cm-1. Mass spectrometric measurement showed a peak at M/Z = 802.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,5-Dibromo-2,6-dimethylnaphthalene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2371812; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 18869-30-2, name is (E)-1,2-Bis(4-bromophenyl)ethene, A new synthetic method of this compound is introduced below., Product Details of 18869-30-2

Step 3: Synthesis of (E)-4,4′-bis[4-(10-phenyl-9-anthryl)phenyl]stilbene; 2.0 g (5.9 mmol) of (E)-4,4′-dibromostilbene, 4.9 g (13 mmol) of 4-(10-phenyl-9-anthryl)phenylboronic acid, 0.053 g (0.24 mmol) of palladium (II) acetate, and 0.25 g (0.83 mmol) of tri(ortho-tolyl)phosphine were put into a 100 mL three-necked flask. Then, the atmosphere in the flask was substituted with nitrogen. 30 mL of ethylene glycol dimethyl ether (abbreviation: DME) and 18 mL (35 mmol) of an aqueous potassium carbonate solution (2.0 mol/L) were added to the mixture and the mixture was refluxed at 90 C. for 6 hours to be reacted. After the reaction was completed, a precipitate in the reaction mixture was collected by suction filtration. The collected precipitate was washed with toluene; then 4.7 g of objective (E)-4,4′-bis[4-(10-phenyl-9-anthryl)phenyl]stilbene (abbreviation: PAP2S) was obtained as a light yellow powdered solid in a yield of 94%. A synthetic scheme of (E)-4,4′-bis[4-(10-phenyl-9-anthryl)phenyl]stilbene is illustrated below (synthetic scheme c-1). A 1H NMR data of the obtained (E)-4,4′-bis[4-(10-phenyl-9-anthryl)phenyl]stilbene is described below. 1H NMR (CDCl3, 300 MHz): delta=7.14-7.21 (m, 2H), 7.30-7.44 (m, 11H), 7.48-7.52 (m, 5H), 7.54-7.61 (m, 8H), 7.63-7.73 (m, 8H), 7.77-7.81 (m, 6H), 7.83-7.91 (m, 4H).The 1H NMR chart is illustrated in each of FIGS. 8A and 8B. It is to be noted that the range of 7.0 to 8.0 ppm in FIG. 8A is expanded and illustrated in FIG. 8B.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Semiconductor Energy Laboratory Co., Ltd.; US2008/81934; (2008); A1;,
Bromide – Wikipedia,
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Related Products of 268733-18-2, A common heterocyclic compound, 268733-18-2, name is 4-Bromo-3,5-bis(trifluoromethyl)aniline, molecular formula is C8H4BrF6N, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

(1)1.0 g of 3,5-bis(trifluoromethyl)-4-bromoaniline was dissolved in 3 mL of hexamethylphosphoric acid triamide, and 730 mg of copper cyanide was added and reacted at 140C for 8 hours under irradiation with microwaves. The reaction solution was left to cool, and then, to the reaction solution, water and ethyl acetate were added, whereupon an insoluble solid content was removed by filtration through cerite. The organic layer was separated, and the aqueous layer was extracted twice with ethyl acetate. The organic layers were put together and washed with a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=5/2) to obtain 550 mg of 3,5-bis(trifluoromethyl)-4-cyanoaniline as white solid.

The synthetic route of 268733-18-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ISHIHARA SANGYO KAISHA, LTD.; EP2172456; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 707-34-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 707-34-6, name is 1,3,5-Tribromoadamantane, This compound has unique chemical properties. The synthetic route is as follows.

A 250 ml three-necked flask equipped with a condenser was charged with 3.7 g (10 mmol) of 1,3,5-tribromoadamantane, 16.0 g of 1,3-dibromo-2-methoxybenzene (60.0 mmol) and30 ml of 1,2-dichloroethane,Condenser duct from the upper end connected to an inverted funnel 30% NaOH aqueous solution,To absorb the HBr produced by the reaction.At 0 ice water bath,1.0 g (ie, 4.0 mmol) of AlBr3 was added to the reaction system,Continue stirring in the ice water bath for half an hour,Then gradually returned to room temperature,The reaction system was heated in an oil bath to 60 C for 5 hours,The reaction solution was cooled to room temperature,Pour into 100 mL of acidic ice water and stir for 1 h.After the ice has completely melted, 100 ml of methylene chloride is added to the mixture for extraction. The organic layer is washed with water until neutral, washed with saturated brine, dried over anhydrous sodium sulfate, filtered and the filtrate is concentrated. The mixture is then recrystallized from a mixed solution of ethyl acetate and methanol ,6.58 g of a white solid was obtained in a yield of 71%.

The chemical industry reduces the impact on the environment during synthesis 1,3,5-Tribromoadamantane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Chinese Academy Of Sciences Physics And Chemistry Technology Institute; Chen Jinping; Li Yi; Yu Tianjun; Zeng Yi; (18 pag.)CN107266319; (2017); A;,
Bromide – Wikipedia,
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Synthetic Route of 927384-44-9, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 927384-44-9, name is 2-(4-Bromophenyl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine, This compound has unique chemical properties. The synthetic route is as follows.

A four-necked flask,4-hydroxy-phenyl boric acid 20.0g (0.15 mol),1,8-diaminonaphthalene protection p- bromophenyl boric acid 46.8g (0.15 mol),Take a potassium carbonate 31.1g (0.23 mol),Ethanol 140mL, was suspended in water 47mL.After the inside the flask was replaced by nitrogen gas,The addition of tetrakistriphenylphosphine palladium (0) 1.7g (1.5 mmol). After the mixture was heated with stirring for 7 hours at 80 ,It was diluted with toluene 300mL,It was separated treated with 5% hydrochloric acid 300mL.The solvent was evaporated,The compound represented by formula (I-60-1) by recrystallizing with acetone / hexane mixed solventIt was obtained 42.9g (0.13 mol).

The chemical industry reduces the impact on the environment during synthesis 2-(4-Bromophenyl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DIC Corporation; Horiguchi, Masahiro; Hayashi, Masanao; Kusumoto, Tetsuo; (63 pag.)JP5962949; (2016); B2;,
Bromide – Wikipedia,
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Electric Literature of 141215-32-9, A common heterocyclic compound, 141215-32-9, name is 4,7-Dibromobenzo[c][1,2,5]thiadiazole-5,6-diamine, molecular formula is C6H4Br2N4S, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Gas in the flask with argon purged 200mL flask,Added1500mg heterocyclic compound according to Journal (Heterocycles), 1992, Vol. 33, No. 1, p.337-348 method described in the manufacture of 3 (1.54mmol), benzil 325mg (1.54mmol), acetic acid 25mL , the flask was immersed in an oil bath heated to 120 deg.] C, and reacted for 2 hours. Subsequently, the flask was cooled to room temperature (25 deg.] C), the reaction mixture was poured into 300mL of methanol. The solid was recovered by filtration, washed with methanol, and dried under vacuum to give 629mg of the title compound 32 (1.26mmol).

The synthetic route of 141215-32-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Co.,Ltd; Ken, Yoshimura; Kenichiro, Oya; (111 pag.)CN105601662; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 89523-51-3, These common heterocyclic compound, 89523-51-3, name is 5-Bromobenzo[c]phenanthrene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Argon atmosphere, 2-nitro-phenylboronic acid 2.00g, 5-bromo-benzo [c] phenanthrene, 6.12g, tetrakis triphenylphosphine palladium (0) 0.462g, DME 80mL, 2M aqueous sodium carbonate solution in the flask was added 40mL and the mixture was heated and stirred 24 hr reflux. after cooling to room temperature (25 ), after the reaction solution was extracted using toluene, and removing the water layer, an organic layer was washed with saturated aqueous sodium chloride. The organic layer was dried over magnesium sulfate, concentrated, and the residue was purified by silica gel column chromatography to give 5- (2-nitro-phenyl) benzo [c] phenanthrene was obtained a 5.72g.

The synthetic route of 89523-51-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Idemitsu Kosan Corporation; Kawamura, Masahiro; Mizuki, Yumiko; Ito, Hirokazu; Hayama, Tomoharu; Haketa, Tasuku; (69 pag.)KR2015/126340; (2015); A;,
Bromide – Wikipedia,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 89523-51-3, name is 5-Bromobenzo[c]phenanthrene, A new synthetic method of this compound is introduced below., COA of Formula: C18H11Br

Example 4 Synthesis of 5-(diphenylamino)benzo[c]phenanthrene 190 mul (1 mmol) of chlorodi-tert-butylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a suspension of 15.3 g (50 mmol) of 5-bromobenzo[c]phenanthrene, 10.2 g (60 mmol) of diphenylamine and 7.7 g (80 mmol) of sodium tert-butoxide in 500 ml of toluene, and the mixture is subsequently heated under reflux for 5 h. After the mixture has been cooled to 60 C., 500 ml of water are added, the organic phase is separated off, filtered through silica gel, evaporated virtually to dryness at 80 C. in vacuo, and 300 ml of ethanol are then added. After cooling, the solid is filtered off with suction. The product is purified by recrystallisation from dioxane five times (about 8 ml/g). Yield: 12.6 g (32 mmol), 64.1%, purity 99.9% (HPLC).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Merck Patent GmbH; US2011/288292; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary