Réaction #3703

Équation de réaction

6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine

SnCl2.2H2O

→

solid

Rendement 102.3%

6,7-Dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine

Rendement 102.3%

Solvants

ethyl alcohol

tetrahydrofuran

Conditions de réaction

Traitement

1. 1
   AutreThe solvents are evaporated in vacuo to a residue which
2. 2
   workup.STIRRINGis stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes
3. 3
   Filtrationfiltered through diatomaceous earth
4. 4
   LavageThe filter pad is washed with 2×10 ml of ethyl acetate
5. 5
   Lavagethe combined extracts washed with brine
6. 6
   Séchagedried (Na2SO4)
7. 7
   Autreevaporated in vacuo

Mode opératoire

To a solution of 0,50 g of 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 10 ml of ethyl alcohol and 2 ml of tetrahydrofuran is added 2.35 g of SnCl2.2H2O and the mixture stirred at 55° C. for 30 minutes. The solvents are evaporated in vacuo to a residue which is stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes and filtered through diatomaceous earth. The filter pad is washed with 2×10 ml of ethyl acetate and the combined extracts washed with brine, dried (Na2SO4) and evaporated in vacuo to give 0.47 g of solid residue which is triturated with ether-hexane to give 0.43 g of light yellow crystalline solid. MS(CI): 338 (M+H, Cl35) 340 (M+H, Cl37)

Source