Ethanol → HCID 59377674、化合物

反応式

[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]

参加物

反応物 3

HCID 702Ethanol

HCID 1118Sulfuric Acid

HCID 59377673HCID 59377673、化合物

生成物 1

HCID 59377674HCID 59377674、化合物

実験手順

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.

後処理

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)

出典と根拠

ORDレコード: ord-c73e3f524fe24ebcb4ed54d7acd43f2e
出典データセット: uspto-grants-2012_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08153808B2

反応ノート

読み込み中…

参加物