반응 #53340

반응 방정식

compound XVIII

(±)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbothiohydrazide

chloroform

methyl isocyanate

→

(±)-1-{8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbothioyl}-4-methyl-semicarbazide

수율 88.0%

반응 조건

후처리

1. 1
   세척After 1 h the reaction mixture was washed with sodium hydrogen carbonate solution and water
2. 2
   농축after concentration the obtained solid material
3. 3
   기타was purified
4. 4
   온도by refluxing in ethanol

실험 절차

To a stirred solution of 0.40 g (1.0 mmol) of compound XVIII in 15 ml of chloroform 0.07 ml (1.2 mmol) of methyl isocyanate was added. After 1 h the reaction mixture was washed with sodium hydrogen carbonate solution and water and after concentration the obtained solid material was purified by refluxing in ethanol. The desired product was 0.36 g, yield: 88%. Mp.: 200° C.

출처