Water → HCID 178457773, 화합물

HRID 1380571노트

반응식

HRID 1380571 반응식
[Cl:1][C:2]1=[C:3]([Cl:9])[C:4]([O:6][C:7]1=[O:8])=[O:5].[CH3:10][CH:11]([CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:17][CH:16]=1)[CH2:12][NH2:13].O>C(O)(=O)C>[CH3:10][CH:11]([CH2:14][C:15]1[CH:16]=[CH:17][C:18]([C:21]([CH3:22])([CH3:24])[CH3:23])=[CH:19][CH:20]=1)[CH2:12][N:13]=[C:4]([OH:5])/[C:3](/[Cl:9])=[C:2](/[Cl:1])\[C:7]([OH:6])=[O:8]

참가 물질

5

반응물 3

HCID 962WaterHCID 70728Dichloromaleic anhydrideHCID 132903003-(4-tert-Butylphenyl)-2-methylpropan-1-amine

생성물 1

HCID 178457773HCID 178457773, 화합물수율 41.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

16.7 g (0.1 mol) of dichloromaleic anhydride and 20.5 g (0.1 mol) of 2-methyl-3-(4-tert.-butylphenyl)-propylamine are stirred in 100 ml of glacial acetic acid under reflux for 4 hours. 100 ml of water are added, the oil which has separated out is extracted with methylene chloride, the methylene chloride phase is concentrated and the residue is recrystallized from ethanol. 14.6 g (41.2% of theory) of dichloromaleic acid N-[2-methyl-3-(4-tert.-butylphenyl)-propyl]-imide of melting point 64°-65° C. are obtained.

후처리

  1. temperatureunder reflux for 4 hours
  2. customthe oil which has separated out
  3. extractionis extracted with methylene chloride
  4. concentrationthe methylene chloride phase is concentrated
  5. customthe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-0757c7d5569f4122929dde6c4dc20450
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04582849

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