Thionyl Chloride → 5-Bromo-2,4-dimethoxybenzoyl chloride

HRID 1967447ノート

反応式

HRID 1967447 の反応式
[Br:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7](O)=[O:8].S(Cl)([Cl:17])=O>C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([O:13][CH3:14])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7]([Cl:17])=[O:8]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 135050975-Bromo-2,4-dimethoxybenzoic acid

生成物 1

HCID 135050985-Bromo-2,4-dimethoxybenzoyl chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
75 °C

実験手順

Under a nitrogen atmosphere, 5-bromo-2,4-dimethoxybenzoic acid (40.0 g) was suspended in toluene solution (DMF concentration: 300 ppm, 200 mL). To the suspension was added dropwise thionyl chloride (21.9 g) at 75° C. After stirring at 75° C. for 1 hr, completion of the reaction was confirmed by HPLC. Toluene and excess thionyl chloride were evaporated under reduced pressure. Toluene (100 mL) was added to the concentrated residue, and the mixture was concentrated again under reduced pressure. THF (100 mL) was added to the obtained 5-bromo-2,4-dimethoxybenzoic acid chloride, which was directly used in the next step.

後処理

  1. customToluene and excess thionyl chloride were evaporated under reduced pressure
  2. additionToluene (100 mL) was added to the concentrated residue
  3. concentrationthe mixture was concentrated again under reduced pressure
  4. additionTHF (100 mL) was added to the obtained 5-bromo-2,4-dimethoxybenzoic acid chloride, which

出典と根拠

ORDレコード
ord-e0e3d20ee74a4a729e4c0e64db93c569
出典データセット
uspto-grants-2013_04
特許番号
US08420821B2

反応ノート

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