Potassium Carbonate → HCID 11293498、化合物

HRID 432079

反応式

HRID 432079 の反応式
[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]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 24083Sulfuric acid magnesium salt (1:1)HCID 9816147Ethyl (2S)-2-ethoxy-3-(4-hydroxyphenyl)propanoateHCID 227084532-(4-Methylsulfonyloxyphenyl)ethylmethanesulfonate2 回

生成物 1

HCID 11293498HCID 11293498、化合物収率 151%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f6c350290544eb0b3dd7b3f74507969
出典データセット
uspto-grants-2003_12
特許番号
US06660879B2

関連ノート

読み込み中…