反应详情

温度

110 °C

A stirred mixture of gamma-valerolactone (40 g.), ethyl 2-(3,4-dichlorophenylamino)-nicotinate (20 g.) and potassium t-butoxide (30 g.) was warmed in an atmosphere of nitrogen to 110° C. and kept there for 5 hr. After cooling somewhat the product was poured into 1000 ml. of 5% KOH solution and was allowed to stir overnight. The basic solution was extracted with ether (2×500 ml.) and the aqueous solution was acidified to pH 5 with conc. HCl. The solid was filtered off, washed with water, dried in air then recrystallized from methanol/charcoal to yield the desired product, m.p. 232°-234° C.

1. temperatureAfter cooling somewhat the product
2. additionwas poured into 1000 ml
3. extractionThe basic solution was extracted with ether (2×500 ml.)
4. filtrationThe solid was filtered off
5. washwashed with water
6. customdried in air
7. customthen recrystallized from methanol/charcoal