Reaktion #53340

Reaktionsgleichung

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

Ausbeute 88.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   WaschenAfter 1 h the reaction mixture was washed with sodium hydrogen carbonate solution and water
2. 2
   Einengenafter concentration the obtained solid material
3. 3
   Sonstigewas purified
4. 4
   Temperaturby refluxing in ethanol

Vorschrift

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.

Quelle