反应详情

To a suspension of 60% sodium hydride (0.65 g) in dry dimethylformamide (20 ml) at 0° C. was added a solution of diethyl 2-(3-chloro-5-trifluoromethyl-2-pyridyl)malonate (5 g) in dry dimethylformamide (10 ml) and the mixture was stirred for 15 minutes. A solution of N-bromomethylphthalimide (3.55 g) in dry dimethylformamide (10 ml) was added dropwise and the mixture was warmed with stirring to 22° C. over 18 hours. Glacial acetic acid (1 ml) was added and the mixture was poured into cold water (500 ml). The aqueous solution was extracted with diethyl ether (3×150 ml) and the combined extract was water washed (3×100 ml). The organic extract was dried (MgSO4) and evaporated to give a crude product. Trituration with diethyl ether/light petroleum (b.p. 40-60° C.) (1:1) gave the title compound, m.p. 159-61° C.

1. temperaturethe mixture was warmed
2. stirringwith stirring to 22° C. over 18 hours
3. extractionThe aqueous solution was extracted with diethyl ether (3×150 ml)
4. extractionthe combined extract
5. washwashed (3×100 ml)
6. extractionThe organic extract
7. dry with materialwas dried (MgSO4)
8. customevaporated
9. customto give a crude product