反应详情

A mixture of 11 parts of 1-[4-fluoro-2-(phenylmethoxy)phenyl]ethanone, 8.48 parts of 3-chlorobenzenecarboperoxoic acid and 260 parts of dichloromethane was stirred for 5 days at room temperature. The precipitate was filtered off and the filtrate was stirred in a saturate thiosulfurate solution for 15 minutes. The organic layer was separated and stirred in a saturate hydrogen carbonate solution for 15 minutes. The organic layer was separated, washed with water, dried, filtered and evaporated. The solid residue was stirred in 240 parts of methanol. 5.3 Parts of sodium methoxide were added portionwise. After complete addition, the whole was stirred for 1 hour at room temperature. After evaporation in vacuo at 50° C., the residue was stirred in water and acidified with a hydrochloric acid solution 3N. Trichloromethane was added, the organic layer was separated, washed twice with water, dried, filtered and evaporated, yielding 10 parts (93%) of 4-fluoro-2-(phenylmethoxy)phenol as a residue (intermediate 77).

1. filtrationThe precipitate was filtered off
2. stirringthe filtrate was stirred in a saturate thiosulfurate solution for 15 minutes
3. customThe organic layer was separated
4. stirringstirred in a saturate hydrogen carbonate solution for 15 minutes
5. customThe organic layer was separated
6. washwashed with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. stirringThe solid residue was stirred in 240 parts of methanol
11. addition5.3 Parts of sodium methoxide were added portionwise
12. additionAfter complete addition
13. stirringthe whole was stirred for 1 hour at room temperature
14. customAfter evaporation in vacuo at 50° C.
15. stirringthe residue was stirred in water
16. additionTrichloromethane was added
17. customthe organic layer was separated
18. washwashed twice with water
19. customdried
20. filtrationfiltered
21. customevaporated