反应详情

A solution of 12.1 g of triethylamine, 4.0 g of malononitrile, and 20 ml of chlorobenzene was added to a slurry of 11.4 g of N-(dichloromethylene)-N,N-diethylammonium chloride and 50 ml of chlorobenzene, at ambient temperature. The reaction temperature was kept below 50° by controlling the rate of addition (time required for complete addition, 30 minutes). After addition, the reaction mixture was stirred for four hours while it returned to ambient temperature. The reaction mixture was filtered and the filtrate concentrated on the rotary evaporator to give a brownish-red liquid. Vacuum distillation gave 3.7 g of liquid 3-chloro-2-cyano-3-(diethylamino)propenenitrile; b.p. 127°-131°/0.05 mm Hg. The ir and nmr spectra were consistent with the assigned structure.

1. customwas kept below 50°
2. additionthe rate of addition (time required for complete addition, 30 minutes)
3. additionAfter addition
4. customreturned to ambient temperature
5. filtrationThe reaction mixture was filtered
6. concentrationthe filtrate concentrated on the rotary evaporator
7. customto give a brownish-red liquid
8. distillationVacuum distillation