反应详情

Chloro-acetyl chloride (3.3 mL, 40.8 mmol) was added with stirring to a solution of the ester of Example 35j (5 g, 13.6 mmol) in CH2Cl2 (100 mL) at 15° C., followed by addition of pyridine (6.6 mL, 81.6 mmol). The reaction mixture was stirred for 2 h, concentrated, treated with water and the solid that precipitated was filtered and purified by refluxing it with stirring in ethyl acetate for 0.5 h. The solid was filtered and dried to obtain the title compound. Yield: 5.5 g, (90.9%); 1H NMR (DMSO-d6): δ 2.7 (s, 3H, CH3), 3.9 (s, 3H, OCH3), 4.31 (s, 2H, CH2), 5.4 (s, 2H, CH2), 7.71 (s, 1H, Ar), 7.98 (s, 1H, Ar), 8.12 (s, 1H, Ar), 8.2 (s, 1H, Ar), 10.77 (s, 1H, Ar); MS: m/e (ES−) 442(M−1).

1. concentrationconcentrated
2. additiontreated with water
3. customthe solid that precipitated
4. filtrationwas filtered
5. custompurified
6. temperatureby refluxing it
7. stirringwith stirring in ethyl acetate for 0.5 h
8. filtrationThe solid was filtered
9. customdried