反应详情

温度

0 °C

Sodium hydride (350 mg) was dissolved in dimethylformamide (10 mL)), and the solution was cooled to 0° C. After addition of tert-butyl methyl malonate (1.52 g), the mixture was stirred for one hour, and the 5-chloro-N,N-dimethyl-2-nitrobenzamide (1.0 g) obtained in Example 2a) was added thereto. The mixture was stirred at 70° C. for 4.5 hours and water was added thereto. The resulting solution was concentrated, diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate and purified by column chromatography on silica gel with ethyl acetate:hexane=1:1 to give the title compound (1.29 g).

1. stirringThe mixture was stirred at 70° C. for 4.5 hours
2. concentrationThe resulting solution was concentrated
3. additiondiluted with ethyl acetate
4. washwashed with water
5. dry with materialThe organic layer was dried over sodium sulfate
6. custompurified by column chromatography on silica gel with ethyl acetate