反応 #53340

反応方程式

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

収率 88.0%

反応条件

後処理

1. 1
   洗浄After 1 h the reaction mixture was washed with sodium hydrogen carbonate solution and water
2. 2
   濃縮after concentration the obtained solid material
3. 3
   その他was purified
4. 4
   温度by refluxing in ethanol

実験手順

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.

出典