반응 #3685

반응 방정식

acetic acid

5,10-dihydro-5-(4-nitro-2-chlorobenzoyl)-4H-pyrazolo[5,1-c][1,4]benzodiazepine

NaHCO3

→

glass

수율 78.7%

5,10-Dihydro-5-(4-amino-2-chlorobenzoyl)-4H-pyrazolo[5,1-c][1,4]benzodiazepine

수율 78.7%

용매

ethanol

반응 조건

후처리

1. 1
   온도is heated at 70°-80° C. for 1 hour
2. 2
   온도The mixture is chilled
3. 3
   추출extracted (several times) with ethyl acetate
4. 4
   건조The combined extracts are dried (Na2SO4)
5. 5
   기타The filtrate is evaporated
6. 6
   workup.DISSOLUTIONthe residue dissolved in dichloromethane
7. 7
   기타The filtrate is evaporated in vacuo

실험 절차

A mixture of 0.553 g of 5,10-dihydro-5-(4-nitro-2-chlorobenzoyl)-4H-pyrazolo[5,1-c][1,4]benzodiazepine, 1.70 g of stannous chloride dihydrate in 20 ml of ethanol is heated at 70°-80° C. for 1 hour. The mixture is chilled, made basic with 1M NaHCO3 and then stirred at room temperature for 0.5 hour. The mixture is brought to pH 5 with acetic acid and extracted (several times) with ethyl acetate. The combined extracts are dried (Na2SO4) and passed through a pad of hydrous magnesium silicate. The filtrate is evaporated and the residue dissolved in dichloromethane and the solution passed through a thin pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo to give 0.40 g of a glass, m.p. 98°-117° C.; Anal. Calc'd: C, 62.9; H, 4.7; N, 16.3; Cl, 11.6. Found: C, 62.4; H, 4.3; N, 15.6; Cl, 11.7.

출처