Réaction #527474

Équation de réaction

1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine

acetic anhydride

→

pure aimed product

Rendement 84.6%

1-(4-Diacetylaminophenyl)-3-acetyl-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine

Rendement 84.6%

Conditions de réaction

Traitement

1. 1
   Autreit was evaporated to dryness under reduced pressure
2. 2
   Filtrationa filter
3. 3
   Lavagewashed with 5×3 ml of water
4. 4
   SéchageAfter drying 2.79 g of the raw triacetyl derivative
5. 5
   Autrewere obtained
6. 6
   LavageAfter washing with 20 ml of isopropanol
7. 7
   Autredrying at 100° C

Mode opératoire

2.0 g (6.7 mmol) of 1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine were refluxed with 40 ml of acetic anhydride for 3 hours, then it was evaporated to dryness under reduced pressure. The crystalline residue was transferred with 25 ml of water to a filter and washed with 5×3 ml of water. After drying 2.79 g of the raw triacetyl derivative were obtained. After washing with 20 ml of isopropanol and drying at 100° C. 2.39 g (84.6%) of the pure aimed product were obtained, m.p. 224°-227° C.

Source