Reaction #53340

Reaction equation

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

Yield 88.0%

Conditions

Workup

1. 1
   WashAfter 1 h the reaction mixture was washed with sodium hydrogen carbonate solution and water
2. 2
   Concentrationafter concentration the obtained solid material
3. 3
   Otherwas purified
4. 4
   Temperatureby refluxing in ethanol

Procedure

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.

Source