تفاعل #710498

معادلة التفاعل

2-chloro-6-(trifluoromethyl)nicotinic acid

BH3-THF

→

[2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol

المذيبات

NaHCO3

THF

ظروف التفاعل

المعالجة

1. 1
   تركيزAfter 16 h the reaction mixture was concentrated under reduced pressure
2. 2
   أخرىto remove THF
3. 3
   أخرىThe resulting reaction mixture
4. 4
   استخلاصextracted with ethyl acetate (2×500 mL)
5. 5
   غسيلThe combined organic layers were washed with water (500 mL), brine (500 mL)
6. 6
   تجفيفdried over anhydrous sodium sulfate
7. 7
   أخرىthe solvent was removed under reduced pressure

الإجراء التجريبي

To a stirred solution of e 2-chloro-6-(trifluoromethyl)nicotinic acid (Int-15) (40 g, 1.0 eq.) in THF (400 mL) was added BH3-THF (266.6 mL, 1.5 eq) at room temperature. The progress of the reaction was monitored by TLC. After 16 h the reaction mixture was concentrated under reduced pressure to remove THF. The resulting reaction mixture was diluted with 10% NaHCO3 (500 mL) and extracted with ethyl acetate (2×500 mL). The combined organic layers were washed with water (500 mL), brine (500 mL), dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure to get crude [2-chloro-6-(trifluoromethyl)pyridin-3-yl]methanol (Int-16) as light yellow liquid, 32 g (85.5%).

المصدر