반응 #9529

반응 방정식

tert-butyl[2-(7-bromo-3-nitroquinolin-4-ylamino)ethyl]carbamate

isopropanol

→

tert-butyl [2-(3-amino-7-bromoquinolin-4-ylamino)ethyl]carbamate

수율 91.1%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타pressure (50 psi, 3.4×105 Pa) overnight
2. 2
   여과The mixture was filtered through a layer of CELITE
3. 3
   여과filter aid
4. 4
   농축the filtrate was concentrated under reduced pressure

실험 절차

A solution of tert-butyl[2-(7-bromo-3-nitroquinolin-4-ylamino)ethyl]carbamate (165.0 g, 401.2 mmol) in acetonitrile (3.3 L) and, isopropanol (990 mL) and 5% platinum on carbon (13.2 g) were added to a Parr vessel, which was placed under hydrogen pressure (50 psi, 3.4×105 Pa) overnight. The mixture was filtered through a layer of CELITE filter aid, and the filtrate was concentrated under reduced pressure to provide 139.29 g of tert-butyl [2-(3-amino-7-bromoquinolin-4-ylamino)ethyl]carbamate as a yellow solid. The product was suspended in a mixture of dichloromethane (4 mL/g) and chloroform (8 mL/g), and the suspension was divided into two equal portions.

출처