Reaktion #53354

Reaktionsgleichung

starting material XVIII

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

chloroacetone

→

title compound

Ausbeute 67.0%

(±)-8-Methyl-7-(5-methyl-6H-1,3,4-thiadiazin-2-yl)-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

Ausbeute 67.0%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationAfter dilution with water the precipitated crystals were filtered off
2. 2
   Sonstigepurified
3. 3
   Temperaturby refluxing in ethyl acetate

Vorschrift

A mixture of 1.00 g (2.50 mmol) of the starting material XVIII, 20 ml of dimethylformamide and 0.57 g (6.16 mmol) of chloroacetone was stirred at room temperature for 2 h. After dilution with water the precipitated crystals were filtered off and purified by refluxing in ethyl acetate to yield 0.73 g (67%) of the title compound; Mp.: 203-204° C.

Quelle