Oxalyl chloride → 3-(3,4-Difluorophenyl)propanoyl chloride

HRID 547657ノート

反応式

HRID 547657 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:9]([CH3:13])C(O)=O)[CH:5]=[CH:6][C:7]=1[F:8].C(Cl)(=O)[C:15]([Cl:17])=[O:16]>CN(C)C=O.ClCCl>[F:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:13][C:15]([Cl:17])=[O:16])[CH:5]=[CH:6][C:7]=1[F:8]

参加物

5

反応物 2

HCID 65578Oxalyl chlorideHCID 20668528444170-17-6

生成物 1

HCID 575859753-(3,4-Difluorophenyl)propanoyl chloride収率 99.8%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

To a dichloromethane solution (200 mL) containing 3,4-difluorophenyl propionic acid (30.45 g, 163.6 mmol) and 2 drops of dimethylformamide was added oxalyl chloride (41.4 g, 327.1 mmol) over 20 min. The resulting solution was stirred for 24 hours at which time the solvent was removed in vacuo. The residual oil was then evaporated with toluene (˜100 mL) yielding 33.4 g of 3-(3,4-difluorophenyl)propanoyl chloride as a yellow liquid, which was taken directly into the next step.

後処理

  1. customwas removed in vacuo
  2. customThe residual oil was then evaporated with toluene (˜100 mL)

出典と根拠

ORDレコード
ord-4b9e394351084ce69d52571f6696f391
出典データセット
uspto-grants-2011_05
特許番号
US07939528B2

反応ノート

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