Thionyl Chloride → 2,5-Dimethoxybenzoyl chloride

HRID 1647317

反応式

HRID 1647317 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5](O)=[O:6].S(Cl)([Cl:16])=O>>[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:4]=1[C:5]([Cl:16])=[O:6]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 760272,5-Dimethoxybenzoic acid

生成物 1

HCID 873642,5-Dimethoxybenzoyl chloride収率 96.7%

実験手順

A mixture of 2,5-dimethoxybenzoic acid (25 g, 137.2 mmol) and thionyl chloride (35 mL, 470.6 mmol) was heated at reflux under Ar for 4 h. The reaction solution was evaporated to dryness and the residue was purified by high vacuum distillation at 127° C./2 mm Hg to give compound 45 as a pale yellow oil (26.5 g, 96.7%). When standing at room temperature, this oil changed to yellow crystals, m.p. 36°-38° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux under Ar for 4 h
  3. customThe reaction solution was evaporated to dryness
  4. distillationthe residue was purified by high vacuum distillation at 127° C./2 mm Hg

出典と根拠

ORDレコード
ord-361308fc52524f648aacc976d313a2e7
出典データセット
uspto-grants-1995_07
特許番号
US05430062

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