Reaktion #53353

Reaktionsgleichung

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

cyclopropylamine

sodium chloride

→

title compound

Ausbeute 87.5%

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

Ausbeute 87.5%

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe precipitated crude product
2. 2
   Extraktionwas extracted into ethyl acetate
3. 3
   WaschenThe solution was washed with water
4. 4
   Sonstigedried
5. 5
   Sonstigeafter evaporation

Vorschrift

A mixture of 5 ml of dimethylformamide, 0.44 g (0.96 mmol) of (±)-7-(5-chloromethyl-1,3,4-thiadiazol-2-yl)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine (Example 34) and 0.37 ml (5.31 mmol) of cyclopropylamine was stirred at 70-80° C. for 1 h. Then the reaction mixture was poured into 20% sodium chloride solution and, the precipitated crude product was extracted into ethyl acetate. The solution was washed with water, dried and after evaporation yielded 0.39 g (85%) of the title compound, as solid foam.

Quelle