反应详情

A solution of acetyl chloride (1.38 g.) in methylene chloride (10 ml.) was added to a mixture of ethyl 2-(2-amino-3-phenoxyphenyl)acetate (4.3 g.), pyridine (1.9 g.) and dried methylene chloride (50 ml.) over 10 minutes at 5° C. with stirring and stirred for 30 minutes at the same temperature. The reaction mixture was concentrated under reduced pressure and to the residue was added 10% hydrochloric acid. The mixture was extracted with ethyl acetate, and the extract was washed with water, dried over magnesium sulfate and then evaporated. The residue was crystallized with a mixture of benzene and n-hexane to give the captioned compound (3.65 g.). mp 106° to 107° C.

1. stirringstirred for 30 minutes at the same temperature
2. concentrationThe reaction mixture was concentrated under reduced pressure and to the residue
3. additionwas added 10% hydrochloric acid
4. extractionThe mixture was extracted with ethyl acetate
5. washthe extract was washed with water
6. dry with materialdried over magnesium sulfate
7. customevaporated
8. customThe residue was crystallized with a mixture of benzene and n-hexane
9. customto give the captioned compound (3.65 g.)