Potassium Carbonate → HCID 11293498, 화합물

HRID 432079노트

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HRID 432079 반응식
[CH3:1][S:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH2:13]CS([O-])(=O)=O)=[CH:8][CH:7]=1)(=[O:4])=[O:3].[CH2:19]([O:21][C:22](=[O:35])[C@@H:23]([O:32][CH2:33][CH3:34])[CH2:24][C:25]1[CH:30]=[CH:29][C:28]([OH:31])=[CH:27][CH:26]=1)[CH3:20].C(=O)([O-])[O-].[K+].[K+].S([O-])([O-])(=O)=O.[Mg+2]>C(#N)C>[CH2:19]([O:21][C:22](=[O:35])[C@@H:23]([O:32][CH2:33][CH3:34])[CH2:24][C:25]1[CH:26]=[CH:27][C:28]([O:31][CH2:13][CH2:12][C:9]2[CH:8]=[CH:7][C:6]([O:5][S:2]([CH3:1])(=[O:3])=[O:4])=[CH:11][CH:10]=2)=[CH:29][CH:30]=1)[CH3:20]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 9816147Ethyl (2S)-2-ethoxy-3-(4-hydroxyphenyl)propanoateHCID 227084532-(4-Methylsulfonyloxyphenyl)ethylmethanesulfonate2회

생성물 1

HCID 11293498HCID 11293498, 화합물수율 151%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of 2-(4-methanesulfonyloxyphenyl)ethylmethanesulfonate (described in Example 1a) (2.41 g; 8.14 mmole) in acetonitrile (11.8 ml) was added to a mixture of (S)-2-ethoxy-3-(4-hydroxyphenyl)propanoic acid ethyl ester (1.3 g; 5.46 mmole), potassium carbonate (2.26 g; 16.4 mmole) and magnesium sulfate (1 g) in acetonitrile (50 ml). The reaction mixture was refluxed for 19 hours. More of 2-(4-methanesulfonyloxyphenyl)ethyl-methanesulfonate (0.8 g; 2.73 mmole) was added and the reaction mixture was refluxed for another 25 hours. Solid material was filtered off and the solvent was evaporated in vacuo to give 3.6 g of (S)-2-ethoxy-3-[4-(2-{4-methanesulfonyloxyphenyl}ethoxy)phenyl]-propanoic acid ethyl ester.

후처리

  1. temperatureThe reaction mixture was refluxed for 19 hours
  2. temperaturethe reaction mixture was refluxed for another 25 hours
  3. filtrationSolid material was filtered off
  4. customthe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-1f6c350290544eb0b3dd7b3f74507969
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660879B2

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