反应详情

A 50 ml. flask equipped with mechanical stirrer and reflux condenser was charged with 19.7 g of ethyl 3-methylamino-4,4,4-trifluoro-2-butenoate and 4.8 g of methylhydrazine and heated to 50°-65° C. for 2.75 hr., then to 40°-45° C. for 2 hr., and then allowed to cool to room temperature and stand overnight. The clear reaction mixture was taken up in 15 ml. of water and conc. hydrochloric acid added dropwise to pH 6.0-6.5 which required 5.2 ml. of acid. The precipitated product was collected by filtration and dried to obtain 7.06 g (42.5%) of product m.p. 127°-128.5° C.

1. customflask equipped with mechanical stirrer
2. temperaturereflux condenser
3. temperatureheated to 50°-65° C. for 2.75 hr
4. waitstand overnight
5. filtrationThe precipitated product was collected by filtration
6. customdried