反应详情

A 12 liter three-necked round-bottomed flask, fitted with a mechanical stirrer, water condenser, nitrogen inlet and bubbler, was charged with 877 g (6 moles) of the potassium salt of 1-hydroxy-2,3-dicyanoprop-1-ene in 61 of anhydrous toluene and 300 ml of anhydrous DMF. To this heterogeneous mixture was added 514 g (6.3 moles) of dimethylamine hydrochloride. The mixture was heated to 80° then cooled to room temperature, filtered and the filter cake rinsed with toluene. The filtrate was concentrated under vacuum to yield 933 g containing on 75% weight, 86% yield of an off which partially crystallized at -5° C. An aliquot of the crystalline portion was collected and recrystallized twice from ether to give white crystals, m.p. 49° C. of 1-(N,N-dimethylamino)-2,3-dicyanoprop-1-ene (CIS 1).

1. customA 12 liter three-necked round-bottomed flask, fitted with a mechanical stirrer, water condenser, nitrogen inlet
2. temperatureThe mixture was heated to 80°
3. filtrationfiltered
4. washthe filter cake rinsed with toluene
5. concentrationThe filtrate was concentrated under vacuum
6. customto yield 933 g
7. additioncontaining on 75% weight, 86% yield of an off which
8. custompartially crystallized at -5° C
9. customAn aliquot of the crystalline portion was collected
10. customrecrystallized twice from ether