Ethanol → 1-Acetyl-4-(2-amino-4-chlorophenyl)-2,3-dihydro-1H-pyrrole-2,2-dicarboxylic acid diethylester

HRID 1390835노트

반응식

HRID 1390835 반응식
[CH2:1]([O:3][C:4]([C:6]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:10][C:9]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[N+:18]([O-])=O)=[CH:8][N:7]1[C:21](=[O:23])[CH3:22])=[O:5])[CH3:2].C(O)C>O1CCCC1.CO.[Pt]>[CH2:1]([O:3][C:4]([C:6]1([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:10][C:9]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[NH2:18])=[CH:8][N:7]1[C:21](=[O:23])[CH3:22])=[O:5])[CH3:2]

참가 물질

6

반응물 2

HCID 702EthanolHCID 128784981-Acetyl-4-(4-chloro-2-nitrophenyl)-2,3-dihydro-1H-pyrrole-2,2-dicarboxylic acid diethyl ester

생성물 1

HCID 128785021-Acetyl-4-(2-amino-4-chlorophenyl)-2,3-dihydro-1H-pyrrole-2,2-dicarboxylic acid diethylester

시약·촉매·용매 3

HCID 23939Platinum촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 82.2 g (0.20 mol) of the compound of Example 10 in 300 ml of tetrahydrofuran and 700 ml of methanol was hydrogenated in the presence of 4 g of 5% sulfided platinum on carbon at room temperature and 1500 psi for 22 hours. The reaction mixture was concentrated and the solid residue (76 g) was recrystallized from ethanol (320 ml) to afford 61.4 g (81%) of light orange crystals, m.p. 151.5-153°. The analytical sample was prepared by a second recrystallization from ethanol: white crystals, m.p, 152-153.5°.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe solid residue (76 g) was recrystallized from ethanol (320 ml)
  3. customto afford 61.4 g (81%) of light orange crystals, m.p. 151.5-153°
  4. customcrystals, m.p, 152-153.5°

출처 및 근거

ORD 기록
ord-f90499345ffe482885377595ef40879b
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04140697

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