Sodium → 2-(4-Hydroxy-5-methoxy-2-methyl-phenoxy)-2-methyl-propionic acid methyl ester

HRID 852429노트

반응식

HRID 852429 반응식
[Na].[CH2:2]([O:4][C:5](=[O:23])[C:6]([O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[C:13]([O:18]C(=O)C)=[CH:12][C:11]=1[CH3:22])([CH3:8])[CH3:7])C>CO>[CH3:2][O:4][C:5](=[O:23])[C:6]([O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[C:13]([OH:18])=[CH:12][C:11]=1[CH3:22])([CH3:8])[CH3:7]

참가 물질

4

반응물 2

HCID 5360545SodiumHCID 674024992-(4-Acetoxy-5-methoxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester

생성물 1

HCID 674032312-(4-Hydroxy-5-methoxy-2-methyl-phenoxy)-2-methyl-propionic acid methyl ester수율 76%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A freshly prepared solution of 91 mg (4 mmol) sodium in 5.4 ml methanol was added within 5 min to an ice cooled solution of 235 mg (0.8 mmol) 2-(4-acetoxy-5-methoxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester in 5.4 ml methanol. The solution was naturally warmed to ambient temperature and after 5 h the solvent was removed under reduced pressure. Ice water/1 M HCl 1/1 was added and the mixture was extracted two times with dichloromethane. The combined extracts were dried over sodium sulfate and the solvent was removed under reduced pressure to yield 153 mg (0.6 mmol, 76%) of the title compound as brown oil which was used in the next step without further purification.

후처리

  1. customwas removed under reduced pressure
  2. additionIce water/1 M HCl 1/1 was added
  3. extractionthe mixture was extracted two times with dichloromethane
  4. dry with materialThe combined extracts were dried over sodium sulfate
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-e5d21fe6fc154c638f37accc94c06c83
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253192B2

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