Thionyl Chloride → 3,5-Dimethoxy-4-(2-propynyloxy)benzoyl chloride

HRID 602012ノート

反応式

HRID 602012 の反応式
[CH2:1]([O:4][C:5]1[C:13]([O:14][CH3:15])=[CH:12][C:8]([C:9](O)=[O:10])=[CH:7][C:6]=1[O:16][CH3:17])[C:2]#[CH:3].S(Cl)([Cl:20])=O>CN(C=O)C.C1(C)C=CC=CC=1>[CH2:1]([O:4][C:5]1[C:13]([O:14][CH3:15])=[CH:12][C:8]([C:9]([Cl:20])=[O:10])=[CH:7][C:6]=1[O:16][CH3:17])[C:2]#[CH:3]

参加物

5

反応物 2

HCID 24386Thionyl ChlorideHCID 131214813,5-Dimethoxy-4-[(prop-2-yn-1-yl)oxy]benzoic acid

生成物 1

HCID 574456693,5-Dimethoxy-4-(2-propynyloxy)benzoyl chloride収率 85.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 1140Toluene溶媒

実験手順

To 100 ml of toluene were added 13.0 g of 4-(2-propynyloxy)-3,5-dimethoxybenzoic acid, 9.5 g of thionyl chloride and 50 mg of DMF and the mixture obtained was heated under reflux for 3 hours. Then, the reaction mixture was concentrated. The solid obtained was washed with hexane to obtain 12.0 g of 4-(2-propynyloxy)-3,5-dimethoxybenzoyl chloride represented by the formula:

後処理

  1. customthe mixture obtained
  2. temperaturewas heated
  3. temperatureunder reflux for 3 hours
  4. concentrationThen, the reaction mixture was concentrated
  5. customThe solid obtained
  6. washwas washed with hexane

出典と根拠

ORDレコード
ord-f63dacc09c7d4a4f95a8a975ee2a7d75
出典データセット
uspto-grants-2011_03
特許番号
US07902400B2

反応ノート

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