反応 #53355

反応方程式

starting material XVIII

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

methyl bromoacetate

→

title compound

収率 37.3%

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

収率 37.3%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   ろ過After dilution with water the precipitated crystals were filtered off
2. 2
   その他purified
3. 3
   温度by refluxing in ethyl acetate

実験手順

A mixture of 1.00 g (2.50 mmol) of the starting material XVIII, 20 ml of dimethylformamide and 0.94 g (6.14 mmol) of methyl bromoacetate was stirred at 70° C. for 1.5 h. After dilution with water the precipitated crystals were filtered off and purified by refluxing in ethyl acetate to yield 0.41 g (37%) of the title compound; Mp.: 294-295° C. (dec.).

出典