Reaktion #53358

Reaktionsgleichung

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

Ausbeute 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

Ausbeute 82.0%

Lösungsmittel

chloroform

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Waschenwashed with sodium hydrogen carbonate solution and water
3. 3
   SonstigeThe residue obtained on concentration
4. 4
   Filtrationfiltered

Vorschrift

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.

Quelle