反应详情

温度

60 °C

Ethanol, (11.0 L), 2-(1-ethoxy-propylidene)-malononitrile, (2.003 kg, 13.34 moles, 1.0 eq), ethyl-2-mercaptoacetate (1.652 kg, 13.34 moles, 1.0 eq.), and potassium acetate (1.983 kg, 20.0 moles, 1.5 eq.) are charged to a 22L 3-neck reaction flask equipped with an addition funnel, thermocouple, overhead stirrer, and condenser. The reaction mixture becomes dark red and exotherms to 72° C. The mixture is stirred for 1.25 hours while cooling to 60° C. Deionized water (2.6 L), is added to the reaction mixture over 30 minutes while cooling to 53° C. The reaction mixture is then cooled to 10° C. over 3.5 hours. The resulting suspension is filtered to recover the precipitate, and the filter cake is rinsed with a chilled mixture of 1.1 L ethanol and 3.9 L water. The filter cake is vacuum dried at room temperature, affording the title compound (2.552 kg) in 85.3% yield.

1. customequipped with an addition funnel
2. customexotherms to 72° C
3. temperaturewhile cooling to 53° C
4. temperatureThe reaction mixture is then cooled to 10° C. over 3.5 hours
5. filtrationThe resulting suspension is filtered
6. customto recover the precipitate
7. washthe filter cake is rinsed with a chilled mixture of 1.1 L ethanol and 3.9 L water
8. customdried at room temperature