反应详情

1-(4-Acetylamino-5-chloro-2-hydroxyphenyl)-5-chloropentan-1-one (1.07 g, 3.5 mmol), potassium carbonate (1.38 g, 10.0 mmol) and iodomethane (0.62 mL, 10.0 mmol) were combined in methyl ethyl ketone (20 mL) and stirred at reflux temperature for 4 hours, 15 minutes. The mixture was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, washed in brine, dried over sodium sulfate, and then evaporated to leave a solid residue. Crystallization of the residue from ethyl acetate-hexanes gave 1-(4-acetylamino-5-chloro-2-methoxyphenyl)-5-chloro-pentan-1-one (0.720 g, 2.37 mmol), m.p. 98°-100° C.

1. temperatureat reflux temperature for 4 hours
2. custom15 minutes
3. customThe mixture was partitioned between ethyl acetate and water
4. customThe ethyl acetate layer was separated
5. washwashed in brine
6. dry with materialdried over sodium sulfate
7. customevaporated
8. customto leave a solid residue
9. customCrystallization of the residue from ethyl acetate-hexanes