Category: 630-17-1

Related Products of 630-17-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 630-17-1 as follows.

Example 21; 2-tert-Butyl-l-[(4,4-difluorocycIohexyl)methyl]-5-{[4-(2,2-dimethyIpropoxy)piperidin- l-yl]carbonyl}-lH-benzimidazole; To a solution of NaH (0.017 g, 0.414 mmol) in 2 mL of DMF at 0C under nitrogen, a DMF solution (2 mL) of l-({2-ter/-butyl-l-[(4,4-difluorocyclohexyl)methyl]-lH-benzimidazol-5- yl}carbonyl)piperidin-4-ol (for preparation, see Example 16, Step B) (0.060 g, 0.138 mmol) was added dropwise. The solution was stirred at O0C under nitrogen for 30 min. 1-Bromo- 2,2-dimethylpropane (0.035 mL, 0.276 mmol) was added dropwise and the solution was stirred at 1000C overnight. The reaction was quenched at 00C by addition of aqueous saturated NaHCOs solution and the solvent was concentrated. The residue was dissolved in EtOAc and washed with saturated aqueous NaHCC>3 solution, brine and dried over anhydrous Na2SO4. The product was purified by reversed-phase HPLC using 20-50% CH3CN/H2O and lyophilized to afford the title compound as the corresponding TFA salt. Yield: 45 mg (53%); 1H NMR (400 MHz, METHANOL-D4) delta 0.89 – 0.93 (m, 9 H), 1.51 – 1.64 (m, 2 H), 1.65 – 1.70 (m, 10 H), 1.70 – 1.85 (m, 6 H), 1.94 (s, 1 H), 2.01 – 2.12 (m, 2 H), 2.20 – 2.32 (m, 1 H), 3.14 (d, /=8.59 Hz, 2 H), 3.32 (s, 1 H), 3.54 – 3.62 (m, 2 H), 3.67 (s, 1 H), 3.93 (s, 1 H), 4.57 (d, /=7.62 Hz, 2 H), 7.62 (dd, /=8.69, 1.46 Hz, 1 H), 7.78 (d, /=0.98 Hz, 1 H), 7.99 (d, /=8.59 Hz, 1 H); MS (ESI) (M+H)+ 504.3.

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; WO2007/145563; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 630-17-1, name is 1-Bromo-2,2-dimethylpropane, 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. name: 1-Bromo-2,2-dimethylpropane

1-neopentyl-4-(4-nitrophenyl)-1H-imidazole To a solution of 4-(4-nitrophenyl)-1H-imidazole (0.500 g, 2.64 mmol) in N,N-dimethylformamide (10 ml) was added cesium carbonate (1.292 g, 3.96 mmol) followed by 1-bromo-2,2-dimethylpropane (0.366 ml, 2.91 mmol). After heating at 850 overnight, the reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried over magnesium sulfate, filtered and concentrated. Normal phase chromatography provided the title compound.

The synthetic route of 1-Bromo-2,2-dimethylpropane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AbbVie Inc.; Hansen, Todd M.; Longenecker, Kenton; Heyman, Howard R.; Curtin, Michael L.; Clark, Richard F.; Sorensen, Bryan; Ji, Zhiqin; Woller, Kevin; Doherty, George; Frey, Robin; (246 pag.)US2017/65575; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 630-17-1 as follows. Safety of 1-Bromo-2,2-dimethylpropane

F) ((2′-fluoro-5′-methoxy-2-neopentyl-[1,1′-biphenyl]-4-yl)oxy)triisopropylsilane Under an argon atmosphere, a solution of 1-bromo-2,2-dimethylpropane (23.2 mL) in diethyl ether (250 mL) was added dropwise to magnesium (4.92 g) at a slow refluxing rate, and the reaction mixture was heated under reflux further for 30 min. Under an argon atmosphere, to a solution of 2′-fluoro-5′-methoxy-4-((triisopropylsilyl)oxy)-[1,1′-biphenyl]-2-yl trifluoromethanesulfonate (19.2 g) and a PEPPSI-SIPr catalyst (trade name) (1.26 g) in THF (200 mL) was added the solution prepared above, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound as a crude oil. This compound was used for the next step without further purification.

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; MIWATASHI, Seiji; SUZUKI, Hideo; OKAWA, Tomohiro; MIYAMOTO, Yasufumi; YAMASAKI, Takeshi; HITOMI, Yuko; HIRATA, Yasuhiro; SHIBUYA, Akito; EP2816023; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 630-17-1, A common heterocyclic compound, 630-17-1, name is 1-Bromo-2,2-dimethylpropane, molecular formula is C5H11Br, 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.

General procedure: (3 mL) was added the electron-deficient alkene (6 mmol) at room temperature. Under vigorous stirring, NiCl2*6H2O (475 mg,2 mmol) was added to the above mixture. The temperature thenrose to 50 C, and stirring was continued for 20 min. The resulting red-brown Ni(0) complex was cooled to room temperature, and a solution of the alkyl bromide (2 mmol) in pyridine (1 mL) was added dropwise. The mixture was stirred for 0.5 h, and then filtered with a short plug (elution with 50 mL of Et2O) and washed with HCl(1N), water and brine, dried over MgSO4, filtered and concentrated. The crude product was purified by flash chromatography on silicagel to afford desired ester products.

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:
Article; Ouyang, Yan; Peng, Yu; Li, Wei-Dong Z.; Tetrahedron; vol. 75; 33; (2019); p. 4486 – 4496;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 630-17-1, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 630-17-1, name is 1-Bromo-2,2-dimethylpropane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

N- (benzyloxycarbonyl) acetamide potassium salt(231 mg, 1.00 mmol) and 18-crown-6 (264 mg, 1.00 mmol)Was dissolved in dimethylformamide (1 mL).After adding 1-bromo-2-chloroethane (83 mL, 1.00 mmol)And the mixture was stirred at room temperature for 19.5 hours.The reaction was terminated by adding saturated aqueous ammonium chloride solution (about 3 mL)The reaction mixture was extracted with ethyl acetate.After washing the organic layer with water and saturated brine,And dried over anhydrous magnesium sulfate.Flash silica gel chromatography(20% ? 40% ethyl acetate / n-hexane)N- (benzyloxycarbonyl) -N- (2-chloroethyl) acetamide(137 mg, 54%) of a colorless oil.

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-Bromo-2,2-dimethylpropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; School corporation Meijo University; Mori, Yuji; Sakai, Takeo; Fukuda, Ayumi; Kasai, Satomi; (28 pag.)JP2018/95576; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 630-17-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 630-17-1 as follows.

(0317) Obtained according to the general method described previously. (0318) Reagents: 3-(2,6-Difluorophenyl)-8-methyl-4-oxo-2-thioxo-1,2,3,4-tetrahydroquinazoline (0.32 mmol, 0.097 g), neopentyl bromide (0.64 mmol, 0.080 mL), K2CO3 (0.0045 g). (0319) The reaction conditions were: 12 hours at ambient temperature. (0320) Purification was carried out by means of silica gel column chromatography (hexane/ethyl acetate, in a ratio of 6:1 by volume). (0321) The yield obtained was: a white solid (51 mg, 42%). P.f.: 152.3 C. 1H-RMN (400 MHz, DMSO) delta: 7.94 (dd, 1H, J=7.9, 0.8 Hz), 7.81-7.73 (m, 2H), 7.49-7.40 (m, 3H), 3.34 (s, 2H), 2.60 (s, 3H), 0.95 (s, 9H). 13C-RMN (100 MHz, DMSO) delta: 160.7, 158.8 (d, 2C, J=252.2 Hz), 156.0, 145.9, 136.9, 135.1, 134.1, 126.9, 125.1, 118.8, 113.5, 44.9, 32.6, 28.9, 17.6, purity analysed by HPLC >99%. EM (m/z): 375 [M+H

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Consejo Superior De lnvestigaciones Cientificas (CSIC); Martinez Gil, Ana; Gil Ayuso-Gontan, Carmen Belen; Perez Fernandez, Daniel Ignacio; Garcia Fernandez, Ana Maria; (22 pag.)US2016/340320; (2016); 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. 630-17-1, name is 1-Bromo-2,2-dimethylpropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C5H11Br

A mixture of 4,5,6,7-tetrahydro-1H-benzo[d]imidazole (5.00 g, 40.9 mmol),90% KOH (3.74 g, 60 mmol) and DMSO (70 mL) was stirred under argon and heated at 40 C for 2 h. After cooling to 10 C, neopentyl bromide (5.5 mL, 44 mmol) was added in one portion, and the resulting mixture was stirred and heated at 40 C for 4 days. The reaction mixture was poured into ice/water (800 mL), treated with 5 NNaOH (200 mL), and extracted with DCM (2 x 400 mL). The extract was washed with water (200 mL), dried over Na2SO4, and the solvent was removed under reduced pressure to give a residue. Column chromatography of the residue (silica gel, ethyl acetate/methanol, 95:5) afforded pure 1-neopentyl-4,5,6,7-tetrahydro-1H- benzo[d]imidazole (4.72 g, 60% yield).

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; NITTO DENKO CORPORATION; STANISLAW, Rachwal; HU, Yufen; ZHANG, Hongxi; WANG, Peng; (42 pag.)WO2018/191238; (2018); 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. 630-17-1, name is 1-Bromo-2,2-dimethylpropane, A new synthetic method of this compound is introduced below., Quality Control of 1-Bromo-2,2-dimethylpropane

Lambda/-(1 -Methylcyclopropyl)-3-((3-methylisoxazol-5-yl)methyl)-2,4-dioxo-1 ,2,3,4- tetrahydroquinazoline-6-sulfonamide (100 mg, 0.260 mmol), cesium carbonate (100 mg, 0.3100 mmol), sodium iodide (8 mg, 0.05 mmol) and 1 -bromo-2,2-dimethylpropane (426 mg, 2.8 mmol) in DMF (2 mL) was heated by microwave irradiation to 130 C for 1 .5 h. The reaction mixture was diluted with water (10 mL) and extracted with EtOAc (2 x 20 mL). The organic phase was combined, washed with brine (10 mL), passed through a hydrophobic frit and evaporated to dryness. The crude product mixture was purified by prep HPLC (high pH) to give the desired product (14 mg, 0.03 mmol, 12%) as an off-white powder

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; CANCER RESEARCH TECHNOLOGY LIMITED; MCGONAGLE, Alison E.; JORDAN, Allan; WASZKOWYCZ, Bohdan; HUTTON, Colin; WADDELL, Ian; HITCHIN, James R.; SMITH, Kate Mary; HAMILTON, Niall M.; (497 pag.)WO2016/92326; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 630-17-1, name is 1-Bromo-2,2-dimethylpropane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: bromides-buliding-blocks

Example 76 [(S)-(3-(4-N-Neopentyl-N-piperazinyl)propylthio)methyl-Sar] -3- [(y-hydroxy)-NMeLeu] – -cyclosporin [0243] [(S)-3-(N-Piperazinylpropylthio)methyl-Sar]-3-[(Y-hydroxy)-N-MeLeu]-4- cyclosporin (150 mg, 0.11 mmol) and neopentyl bromide (MW 151.05, d 1.195, 136 mu, 1.08 mmol) were dissolved in dichloromethane (20 ml), followed by adding sodium carbonate (MW: 105.99, 28.6 mg, 0.27 mmol). The mixture was stirred at room temperature overnight. Then the reaction mixture was washed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by chromatography on silica gel using dichloromethane and methanol as eluent to give product [Molecular Formula: C75H137N13O13S; Exact Mass: 1460.02; MS (m/z): 1460.64 (M+l)+, 1482.72 (M+Na)+; TLC Rf: 0.43 (dichloromethane/methanol = 9: 1); HPLC RT: 11.25 min (C8 reverse phase column: 250 mm; acetonitrile/water (0.05% trifluoroacetic acid); operation temperature: 64 C; detector: 210 nm)].

The synthetic route of 630-17-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SU, Zhuang; LONG, Zhengyu; YANG, Suizhou; WO2014/145686; (2014); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 630-17-1, name is 1-Bromo-2,2-dimethylpropane, 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 630-17-1, Quality Control of 1-Bromo-2,2-dimethylpropane

Intermediate 7A: 6-{(E)-2-[3-(Difluoromethoxy)-2-(2,2-dimethylpropoxy)phenyl]vinyl}imidazo[2,1-b][1,3]thiazole-5-carboxylic acid; Step 1 Ethyl 6-{(E)-2-[3-(difluoromethoxy)-2-(2,2-dimethylpropoxy)phenyl]vinyl}imidazo[2,1-b][1,3]thiazole-5-carboxylate: To a stirred solution of Intermediate 6 (1.60 g, 4.209 mmol) in anhydrous N,N-dimethylformamide (10 mL) was added cesium carbonate (2.74 g, 8.418 mmol) followed by 1-bromo-2,2-dimethylpropane (1.60 mL, 12.629 mmol) at room temperature. The resulting suspension was stirred at 110 C. overnight under nitrogen atmosphere. The reaction mixture was cooled to room temperature and diluted with ethyl acetate (200 mL) and water (100 mL). The layers were separated. Aqueous layer was extracted with ethyl acetate (2×50 mL) and the combined organic layers were washed with brine (2×50 mL), dried (Na2SO4) and filtered. The filtrate was concentrated under reduced pressure. The residue obtained after the evaporation of the solvent was purified by silica gel column chromatography using 10% ethyl acetate in petroleum ether to obtain 1.20 g of the product as an off-white solid; 1H NMR (300 MHz, DMSO-d6) delta 1.07 (s, 9H), 1.39 (t, J=6.9 Hz, 3H), 3.57 (s, 2H), 4.35-4.42 (m, 2H), 7.18 (t, J=74.7 Hz, 1H), 7.20-7.25 (m, 2H), 7.47 (d, J=3.9 Hz, 1H), 7.52-7.58 (m, 1H), 7.73 (d, J=16.2 Hz, 1H), 7.90 (d, J=16.2 Hz, 1H), 8.10-8.16 (m, 1H); APCI-MS (m/z) 451.10 (MH)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,2-dimethylpropane, and friends who are interested can also refer to it.

Reference:
Patent; Glenmark Pharmaceuticals S.A; US2010/152192; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary