6-Bromo-4-fluoro-1-isopropyl-2-methyl-1H-benzo[d]imidazole synthesis
- Product Name:6-Bromo-4-fluoro-1-isopropyl-2-methyl-1H-benzo[d]imidazole
- CAS Number:1231930-33-8
- Molecular formula:C11H12BrFN2
- Molecular Weight:271.13
1301214-70-9
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1231930-33-8
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Yield:1231930-33-8 80%
Reaction Conditions:
with sodium tetrahydroborate at 50; for 4 h;
Steps:
1.2
(2) In a 2L clean four-necked flask equipped with stirring, thermometer and condenser,Pour into the organic phase separated in the previous step, add 110g (1.90mol) of acetone, turn on the stirring, and stir evenly.Then add 340g (1.61mol) of sodium acetate borohydride in batches and raise the temperature to 50°C in an oil bath, keep the temperature for 4 hours,The reaction was monitored by TLC. The developing solvent was (dichloromethane: methanol = 20:1). After the reaction, it was cooled to room temperature and poured into a separatory funnel. The water produced by the reaction was separated and washed twice with 200 g of water. The upper layer was organic The phase is concentrated to dryness,The yellow solid obtained is the crude product. Add n-heptane with twice the mass ratio to recrystallize, cool to 5°C and crystallize for two hours, and filter to318 g of a pale yellow to off-white product was obtained, the total yield was 80%, and the liquid phase purity was 99%.
References:
Jinan Wu Tong Biological Technology Co., Ltd.;Wang Yunguang;Li Xin;Mao Zhehui;Zhong Daohuang;Zhang Xumeng CN112028834, 2020, A Location in patent:Paragraph 0039; 0041
1231930-29-2
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1231930-33-8
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1118-69-0
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1231930-33-8
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67567-26-4
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1231930-33-8
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42717-36-2
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1231930-33-8
218 suppliers
$13.00/100mg