反应详情

温度

-5 °C

102.3 g (0.72 mol) Dimethyl acetylenedicarboxylate was added to 1000 ml ether and the mixture cooled to -5° C. in an ice-methanol bath. 33 g (0.72 mol) methylhydrazine in 100 ml ether was added dropwise at a rate that the inner temperature did not rise above 0° C. The mixture was stirred for one hour at 0° C., the precipitate suction filtered off, washed with ether and dried at 40° C. in vacuo. The intermediate was immersed in an oil-bath heated to 120° C. The reaction product was recrystallised from methanol.

1. customdid not rise above 0° C
2. filtrationthe precipitate suction filtered off
3. washwashed with ether
4. customdried at 40° C. in vacuo
5. customThe intermediate was immersed in an oil-bath
6. temperatureheated to 120° C
7. customThe reaction product was recrystallised from methanol