Ethanol → HCID 59377674, 화합물

반응식

[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([OH:9])=[CH:4][C:3]=1[CH2:10][C:11]([OH:13])=[O:12].S(=O)(=O)(O)O.[CH3:19][CH2:20]O>>[CH2:19]([O:12][C:11](=[O:13])[CH2:10][C:3]1[CH:4]=[C:5]([OH:9])[C:6]([F:8])=[CH:7][C:2]=1[Br:1])[CH3:20]

참가 물질

반응물 3

HCID 702Ethanol

HCID 1118Sulfuric Acid

HCID 59377673HCID 59377673, 화합물

생성물 1

HCID 59377674HCID 59377674, 화합물

실험 절차

To a solution of (2-bromo-4-fluoro-5-hydroxy-phenyl)-acetic acid (5.06 g) in EtOH (100 ml) was added sulfuric acid (0.2 ml) and the mixture was stirred at room temperature for 24 hours. The mixture was heated at 70° C. with stirring for an additional 24 h. The mixture was evaporated to dryness under reduced pressure. Purification of the residue by flash chromatography (hexanes:EtOAc/9:1) gave (2-bromo-4-fluoro-5-hydroxy-phenyl)-acetic acid ethyl ester (4.66 g) as a solid.

후처리

temperatureThe mixture was heated at 70° C.
stirringwith stirring for an additional 24 h
customThe mixture was evaporated to dryness under reduced pressure
customPurification of the residue by flash chromatography (hexanes:EtOAc/9:1)

출처 및 근거

ORD 기록: ord-c73e3f524fe24ebcb4ed54d7acd43f2e
출처 데이터셋: uspto-grants-2012_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08153808B2

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