Methanol → Benzoic acid, 5-chloro-4-hydroxy-2-methoxy-, methyl ester

HRID 630397ノート

反応式

HRID 630397 の反応式
[Cl:1][C:2]1[C:3]([OH:13])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[CH3:14]O>C(Cl)(=O)C>[Cl:1][C:2]1[C:3]([OH:13])=[CH:4][C:5]([O:11][CH3:12])=[C:6]([CH:10]=1)[C:7]([O:9][CH3:14])=[O:8]

参加物

4

反応物 2

HCID 887MethanolHCID 150967495-Chloro-4-hydroxy-2-methoxybenzoic acid2 回

生成物 1

HCID 21536136Benzoic acid, 5-chloro-4-hydroxy-2-methoxy-, methyl ester収率 75%

試薬・触媒・溶媒 1

HCID 6367Acetyl chloride溶媒

反応条件

温度
60 °C

実験手順

To a solution of 5-chloro-4-hydroxy-2-methoxybenzoic acid (intermediate 52; 4.17 g; 13.69 mmol) in 123 ml of anhydrous methanol, 2.2 ml of acetyl chloride were added. The solution was stirred at 60° C. under nitrogen atmosphere for 18 hrs. The solution was evaporated under reduced pressure and the residue purified by preparative reversed-phase HPLC (Cl2CH2/EtOAc from 100/0 to 80/20), affording 2.2 g (75%) of a red solid.

後処理

  1. customThe solution was evaporated under reduced pressure
  2. customthe residue purified by preparative reversed-phase HPLC (Cl2CH2/EtOAc from 100/0 to 80/20)

出典と根拠

ORDレコード
ord-98eb09ede37c4cbd8b72991854687cba
出典データセット
uspto-grants-2016_04
特許番号
US09315463B2

反応ノート

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