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

HRID 630397노트

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HRID 630397 반응식
[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]

참가 물질

4

반응물 2

HCID 887MethanolHCID 150967495-Chloro-4-hydroxy-2-methoxybenzoic acid2회

생성물 1

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

시약·촉매·용매 1

HCID 6367Acetyl chloride용매

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온도
60 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-98eb09ede37c4cbd8b72991854687cba
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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