反应详情

A mixture of 0.524 g (0.002 mole) of 3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide and 1.5 ml of formic acetic anhydride (prepared by reacting sodium formate and acetyl chloride in ether at 23°-27° C. for 5.5 hr, filtering and evaporating off the ether) was stirred at room temperature for about 54 hr. The mixture was evaporated to dryness and the residue was partitioned between 7 ml methylene chloride and 2 ml water. The methylene chloride layer was separated, dried over sodium sulfate and evaporated to dryness. The residue was triturated with ether and the mixture subjected to filtration to give a solid white filter cake weighing 0.398 g after drying. The solid was stirred with more ether for 10 minutes and the mixture filtered to give 0.350 g (61%) white powder, m.p. 117.5°-119° C.

1. customprepared
2. customat 23°-27° C.
3. customfor 5.5 hr
4. filtrationfiltering
5. customevaporating off the ether)
6. customThe mixture was evaporated to dryness
7. customthe residue was partitioned between 7 ml methylene chloride and 2 ml water
8. customThe methylene chloride layer was separated
9. dry with materialdried over sodium sulfate
10. customevaporated to dryness
11. customThe residue was triturated with ether
12. filtrationthe mixture subjected to filtration
13. customto give a solid white filter cake
14. customafter drying
15. stirringThe solid was stirred with more ether for 10 minutes
16. filtrationthe mixture filtered