Category: 101417-40-7

Synthetic Route of 101417-40-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 101417-40-7 name is 4-(Bromomethyl)benzo[d][1,3]dioxole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

5.8 g (0.025 mol) of Va, 3.3 g (0.027 mol) of p-hydroxybenzaldehyde,10.2 g (0.076 mol) of potassium carbonate and 1 g of potassium iodide were added to 40 ml of acetone and the reaction was refluxed overnight.Stop the reaction, filter, evaporate the solvent under reduced pressure, add ethyl acetate and water, and separate the liquid.The aqueous phase was extracted with ethyl acetate and the organic phases were combined, washed with saturated brine and dried over anhydrous sodium sulfate for 8 hours.The desiccant was filtered off, the solvent was evaporated under reduced pressure, and the residue was separated by silica gel column chromatography.Elution with petroleum ether:ethyl acetate (10:1) to collect the desired components,VIb white solid 5.1g, yield 78.2%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(Bromomethyl)benzo[d][1,3]dioxole, and friends who are interested can also refer to it.

Reference:
Patent; The Chinese People’s Liberation Army Military Academy Of Medical Sciences Poison Pharmaceutical Institute; Zhong Bohua; Zhang Ping; He Xinhua; Shi Weiguo; Fan Shiyong; Yao Yishan; Jia Hongxin; (20 pag.)CN103804341; (2018); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 101417-40-7, 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. 101417-40-7, name is 4-(Bromomethyl)benzo[d][1,3]dioxole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2,4-dimethyl-N-(4-(2-oxo-1,2,3,4-tetrahydroquinolin-6-yl)thiazol-2-yl)oxazole-5-carboxamide (0.050 g, 0.136 mmol) in anhydrous dimethylformamide (3 mL) in a flamed dried flask under argon atmosphere at 0 C. was added sodium hydride (60% in mineral oil, 0.014 g, 0.339 mmol) was added in one portion. The reaction was stirred for 10 min at 0 C. then 4-(bromomethyl)benzo[d][1,3]diozole (0.031 g, 0.142 mmol) was added as a solid in one portion. The mixture was stirred for 90 minutes, then 1 hour at room temperature. After consumption of starting material, the reaction mixture was quenched with saturated ammonium chloride (25 mL) and extracted with ethyl acetate (2*25 mL). The combined organics were washed once with saturated sodium bicarbonate (50 mL) and dried over anhydrous sodium sulfate. The concentrated residue was purified by flash chromatography over silica gel using 95:5 dichloromethane/methanol to give N-(4-(1-(benzo[d][1,3]dioxol-4-ylmethyl)-2-oxo-1,2,3,4-tetrahydroquinolin-6-yl)thiazol-2-yl)-2,4-dimethyloxazole-5-carboxamide (0.063 g, 92%) as light yellow solid. 1H NMR (400 MHz, DMSO-d): delta 12.52 (s, 1H), 7.80 (d, 1H, J=1.6 Hz), 7.70 (dd, 1H, J=8.4, 2.0 Hz), 7.56 (bs, 1H), 6.97 (d, 1H, J=8.4 Hz), 6.80 (dd, 1H, J=8.0, 1.6 Hz), 6.75 (m, 1H), 6.59 (dd, 1H, J=8.0, 1.6 Hz), 6.05 (s, 2H), 5.10 (s, 2H), 2.99 (m, 2H), 2.71 (m, 2H), 2.48 (s, 3H), 2.40 (s, 3H). MS (ESI): Calcd. for C26H22N4O5S: 502, found 503 (M+1)+.

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, 4-(Bromomethyl)benzo[d][1,3]dioxole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nantbio, Inc.; Tao, Chunlin; Nallan, Laxman; Ho, David G.; Wang, Qinwei; Weingarten, Paul; Juncker-Jensen, Anna B.; (121 pag.)US2018/201610; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 101417-40-7, name is 4-(Bromomethyl)benzo[d][1,3]dioxole, 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 101417-40-7, Quality Control of 4-(Bromomethyl)benzo[d][1,3]dioxole

7.5 g (0.033 mol) of 2,3-dimethoxymethylene benzyl bromide,4.5 g (0.036 mol) of m-hydroxybenzaldehyde and 13.5 g (0.099 mol) of potassium carbonate were dissolved in 80 ml of DMF.The reaction was stirred overnight at 40C. After the reaction was stopped, it was filtered after the temperature was lowered to room temperature.An equal volume of water and ethyl acetate were added to the filtrate and the layers were separated. The aqueous phase was extracted twice with ethyl acetate.The organic phases were combined and washed in the order of saturated sodium bicarbonate solution-water-saturated brine.Anhydrous sodium sulfate was dried for 8 h. The desiccant was filtered off, the solvent was evaporated under reduced pressure, and the residue was separated by silica gel column chromatography.Elution with petroleum ether:ethyl acetate (10:1) to collect the desired components,Evaporation under reduced pressure gave a white solid VId 6.3 g, yield 74.8%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(Bromomethyl)benzo[d][1,3]dioxole, and friends who are interested can also refer to it.

Reference:
Patent; The Chinese People’s Liberation Army Military Academy Of Medical Sciences Poison Pharmaceutical Institute; Zhong Bohua; Zhang Ping; He Xinhua; Shi Weiguo; Fan Shiyong; Yao Yishan; Jia Hongxin; (20 pag.)CN103804341; (2018); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 101417-40-7, 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. 101417-40-7, name is 4-(Bromomethyl)benzo[d][1,3]dioxole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

a 1,3-Benzodioxole-4-methanethiol The subtitled compound (0.29 g) was prepared by the method of Example 6, step (c) using 4-(bromomethyl)-1,3-benzodioxole (0.51 g). MS (EI) 168 (M+), 135 (100%).

The synthetic route of 4-(Bromomethyl)benzo[d][1,3]dioxole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bonnert, Roger; Gardiner, Stewart; Hunt, Fraser; Walters, Iain; US2003/55250; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary