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Water → 2-(2-Bromo-3-methylbutyryl)aminophenol

HRID 622372
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HRID 622372 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8].C(=O)([O-])O.[Na+].O.[Br:15][CH:16]([CH:20]([CH3:22])[CH3:21])[C:17](Cl)=[O:18]>C(OCC)(=O)C>[Br:15][CH:16]([CH:20]([CH3:22])[CH3:21])[C:17]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[OH:8])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 58012-AminophenolHCID 516892Sodium BicarbonateHCID 124869822-Bromo-3-methylbutanoyl chloride

생성물 1

HCID 142346662-(2-Bromo-3-methylbutyryl)aminophenol

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a mixture of 2-aminophenol (27 25 g), sodium hydrogencarbonate (31.5 g), ethyl acetate (250 ml), and water (200 ml), a solution of 2-bromo-3-methylbutyryl chloride (49.8 g) in ethyl acetate (100 ml) was added dropwise with ice-cooling and with stirring. After stirring with ice-cooling for further 1 hour, the ethyl acetate layer was separated, washed with water, and dried (MgSO4), and the solvent was evaporated off. The residue was crystallized from hexane, to give 2-(2-bromo-3-methylbutyryl)aminophenol. Yield was 59.7 g (87.9%). Recrystallization from isopropyl ether gave colorless prisms, mp 110°-111° C.

후처리

  1. temperaturecooling
  2. stirringAfter stirring with ice-
  3. temperaturecooling for further 1 hour
  4. customthe ethyl acetate layer was separated
  5. washwashed with water
  6. dry with materialdried (MgSO4)
  7. customthe solvent was evaporated off
  8. customThe residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-3cdf2d7774da4f11af7102dc3fd8608c
출처 데이터셋
uspto-grants-1988_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04771050

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