반응 #74462

반응 방정식

5-bromo-2-chlorobenzoic acid

compound 3

5-bromo-2-chlorobenzoic acid

→

title compound

5-Bromo-2-chlorobenzyl alcohol

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도re-cooled to 0° C.
2. 2
   기타quenched with methanol
3. 3
   workup.ADDITIONThe mixture was diluted with water
4. 4
   추출extracted with ethyl acetate
5. 5
   세척The organic layer was washed with brine
6. 6
   건조dried over magnesium sulfate
7. 7
   여과filtered
8. 8
   기타evaporated in vacuo

실험 절차

To a solution 5-bromo-2-chlorobenzoic acid (compound 3, 100 g, 425 mmol) in tetrahydrofuran (500 mL) at 0° C. was added borane dimethyl sulfide complex (170 mL, 170 mmol). The resulting mixture was stirred with gradual warming to ambient temperature over 15 h, re-cooled to 0° C., and quenched with methanol. The mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, filtered and evaporated in vacuo to yield the title compound as a white solid, which was used without further purification.

출처