反应详情

温度

130 °C

A suspension of 55 gm of 7-chloro-5-(2'-chlorophenyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one in 85 ml of N,N-dimethyl-formamide diethylacetal was heated to 130°C in a vessel equipped with a descending condenser, whereby a clear solution was formed after a short time. The temperature of the reaction solution was maintained at 130°C for 41 hours, during which time the ethanol formed by the reaction slowly distilled over. Thereafter, the reaction solution was cooled to about 80°C and then admixed with 50 ml of isopropanol. Upon further cooling of the mixture, a reddish-orange crystalline substance separated out which was collected by vacuum filtration, washed with petroleum ether and recrystallized from isopropanol, whereupon it had a melting point of 202°-203°C. It was identified to be the compound of the formula ##SPC5##

1. customequipped with a descending condenser
2. customwhereby a clear solution was formed after a short time
3. customformed by the reaction
4. distillationslowly distilled over
5. temperatureThereafter, the reaction solution was cooled to about 80°C
6. temperatureUpon further cooling of the mixture
7. customa reddish-orange crystalline substance separated out which
8. filtrationwas collected by vacuum filtration
9. washwashed with petroleum ether
10. customrecrystallized from isopropanol, whereupon it