反応 #53358

反応方程式

methanol

starting material XXVII

(±)-1-Methyl-3-{8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbothioyl}-urea

bromine

→

title compound

収率 82.0%

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

収率 82.0%

溶媒

chloroform

chloroform

chloroform

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   洗浄washed with sodium hydrogen carbonate solution and water
3. 3
   その他The residue obtained on concentration
4. 4
   ろ過filtered

実験手順

To an ice cooled stirred solution of 0.44 g (1.0 mmol) of the starting material XXVII in 8 ml of chloroform a solution of 0.19 g (1.2 mmol) of bromine in 3 ml of chloroform was added. After 0.5 h the reaction mixture was diluted with 15 ml of chloroform and washed with sodium hydrogen carbonate solution and water. The residue obtained on concentration was stirred with methanol and filtered to yield 0.36 g (82%) of the title compound. Mp.: 296° C. after recrystallization from ethyl acetate.

出典