反应详情

温度

65 °C

Tert-butyl nitrite (0.547 ml, 4.6 mmol) is dissolved in 5 ml of dimethylformamide and heated to 65° C. A solution of 155 (1.5 g, 4.6 mmol) in 5 ml of dimethylformamide is added dropwise and the mixture is stirred of additional 10 minutes. The brown solution is cooled to room temperature, diluted with diethyl ether and washed with 2N HCl and brine. The organic layers are dried over sodium sulphate and evaporated. The crude product (1.5 g of a brown oil) is further purified by flash-chromatography (hexane/ethyl acetate 9:1).

1. temperatureThe brown solution is cooled to room temperature
2. washwashed with 2N HCl and brine
3. dry with materialThe organic layers are dried over sodium sulphate
4. customevaporated
5. customThe crude product (1.5 g of a brown oil) is further purified by flash-chromatography (hexane/ethyl acetate 9:1)