Benzene → Bromobutide

HRID 1577469

반응식

HRID 1577469 반응식
[Br:1][CH:2]([C:6]([CH3:9])([CH3:8])[CH3:7])[C:3](O)=[O:4].C1C=CC=CC=1.[CH3:16][C:17]([NH2:25])([CH3:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C1(N=C=NC2CCCCC2)CCCCC1>N1C=CC=CC=1>[CH3:16][C:17]([NH:25][C:3](=[O:4])[CH:2]([C:6]([CH3:9])([CH3:8])[CH3:7])[Br:1])([CH3:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

6

반응물 4

HCID 241BenzeneHCID 10868DicyclohexylcarbodiimideHCID 68509CumylamineHCID 1842512-Bromo-3,3-dimethylbutanoic Acid

생성물 1

HCID 53079Bromobutide수율 68.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Into a 200 ml four-necked flask, there were charged α-bromo-tert-butylacetic acid (9.8 g) and benzene (50 ml), and pyridine (50 ml) and α,α-dimethylbenzylamine (6.9 g) were dropwise added thereto while stirring at room temperature. Dicyclohexylcarbodiimide (10.8 g) was further added thereto, and the reaction was continued at 60°-70° C. for 6 hours, followed by cooling. The solvent was distilled off under reduced pressure, and the residue was extracted with hot benzene. The benzene extract was concentrated by distillation, and the residue was recrystallized from ethanol to give N-(α,α-dimethylbenzyl)-α-bromo-tert-butylacetamide (10.8 g).

후처리

  1. additionwere dropwise added
  2. temperatureby cooling
  3. distillationThe solvent was distilled off under reduced pressure
  4. extractionthe residue was extracted with hot benzene
  5. extractionThe benzene extract
  6. concentrationwas concentrated by distillation
  7. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-f5fd1af2f93548e8849b7c91813b75d6
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04288244

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