反应详情

温度

115 °C

A mixture of diethyl {[(1-ethyl-1H-pyrazol-5-yl)amino]methylene}malonate (2.5 g, 0.009 mole) and phosphorous oxy chloride (17.7 ml, 0.185 mole) was heated at 110-120° C. under stirring for about 3 hours under argon atmosphere. The reaction mixture was poured into ice water. It was extracted with dichloromethane and washed with brine. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo to give pure white solid compound. Yield: 1.8 g. m/z: (M++1) 253.9.

1. extractionIt was extracted with dichloromethane
2. washwashed with brine
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customto give pure white solid compound