反应详情

温度

15 °C

Alternatively the title compound may be prepared by the following procedure. Charge ethanol (3.40 L, denatured with 0.5% toluene) to a 22 L 3-neck reaction flask equipped with a mechanical stirrer, condenser, addition funnel and cooling bath. Cool the ethanol to 8° C. and add sodium ethoxide (805 grams, 11.35 mol) portion-wise over 20 minutes. In a separate flask, combine sarcosine ethyl ester hydrochloride (697 g, 4.54 mol), 2-(1-ethoxy-propylidene)-malononitrile (681 grams, 4.54 mol, prepared in preparation 35) and ethanol (3.0 L) and stir to dissolve the solids. Add the resulting solution to the 22 L flask over 33 minutes while maintaining about 11 C. Maintain the reaction mixture between 10-20° C. for 3.5 hours. Stir the mixture at room temperature overnight, then cool to 1° C. Adjust the pH to 7.0 by adding 1 N HCl (6.58 L) and stir the resulting suspension at 0-5° C. for 3 hours. Collect the precipitate by filtration, rinse the filter cake with deionized water (1.0 L) and vacuum-dry at 40° C., to afford the title compound in 66.7% yield. Mass spectrum (m/e): 222.4 (M+1).

1. temperaturecooling bath
2. customIn a separate flask, combine
3. dissolutionto dissolve the solids
4. additionAdd the resulting solution to the 22 L flask over 33 minutes
5. temperaturewhile maintaining about 11 C
6. temperaturecool to 1° C
7. stirringstir the resulting suspension at 0-5° C. for 3 hours
8. customCollect the precipitate
9. filtrationby filtration
10. washrinse the filter cake with deionized water (1.0 L)
11. customvacuum-dry at 40° C.