Reaktion #3613

Reaktionsgleichung

10,11-dihydro-10-(3-methyl-4-nitro-benzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

hydrazine

→

desired product

Ausbeute 85.2%

10,11-Dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

Ausbeute 85.2%

Lösungsmittel

ethyl alcohol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated on a steam bath for 1 hour
2. 2
   FiltrationThe reaction mixture is filtered hot through diatomaceous earth
3. 3
   Sonstigeevaporated in vacuo to a residue
4. 4
   SonstigeThe residue is crystallized from methylene chloride-hexane

Vorschrift

A mixture of 1.22 g 10,11-dihydro-10-(3-methyl-4-nitro-benzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.2 g of 10% Pd/C and 0.35 g of anhydrous hydrazine in 50 ml of absolute ethyl alcohol is heated on a steam bath for 1 hour. The reaction mixture is filtered hot through diatomaceous earth and evaporated in vacuo to a residue. The residue is crystallized from methylene chloride-hexane to give 0.95 g of the desired product as crystals, m.p. 232°-234° C.

Quelle