Water → 2-Ethoxy-3-(4-{2-[4-(2-propanesulfonyloxy)phenyl]ethoxy}phenyl)propanoic acid ethyl ester

HRID 987253ノート

反応式

HRID 987253 の反応式
C(N(CC)CC)C.[CH2:8]([O:10][C:11](=[O:33])[CH:12]([O:30][CH2:31][CH3:32])[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=2)=[CH:16][CH:15]=1)[CH3:9].[CH:34]([S:37](Cl)(=[O:39])=[O:38])([CH3:36])[CH3:35].O>ClCCl>[CH2:8]([O:10][C:11](=[O:33])[CH:12]([O:30][CH2:31][CH3:32])[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][C:23]2[CH:24]=[CH:25][C:26]([O:29][S:37]([CH:34]([CH3:36])[CH3:35])(=[O:39])=[O:38])=[CH:27][CH:28]=2)=[CH:16][CH:15]=1)[CH3:9]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 824082-Propanesulfonyl chlorideHCID 54239207HCID 54239207、化合物

生成物 1

HCID 865950602-Ethoxy-3-(4-{2-[4-(2-propanesulfonyloxy)phenyl]ethoxy}phenyl)propanoic acid ethyl ester収率 90.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Triethylamine (0.64 g; 6.28 mmole) was slowly added to a solution of 2-ethoxy-3-{4-[2-(4-hydroxyphenyl)ethoxy]phenyl}propanoic acid ethyl ester (1.5 g; 4.18 mmole) in dry dichloromethane (20 ml). After cooling to 0° C. isopropylsulfonyl chloride (0.9 g; 6.28 mmole) was added slowly. The reaction mixture was stirred over night at room temperature, water was added and the mixture was extracted with dichloromethane. The organic phase was washed with hydrochloric acid (1M) and sodium bicarbonate solution, dried (magnesium sulfate) and evaporated in vacuo to give 1.75 g (yield 90%) of 2-ethoxy-3-(4-{2-[4-(2-propanesulfonyloxy)phenyl]ethoxy}phenyl)propanoic acid ethyl ester.

後処理

  1. additionwas added slowly
  2. extractionthe mixture was extracted with dichloromethane
  3. washThe organic phase was washed with hydrochloric acid (1M) and sodium bicarbonate solution
  4. dry with materialdried (magnesium sulfate)
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-4fdfdc209e8c45d3a1980db436027294
出典データセット
uspto-grants-2003_10
特許番号
US06630600B1

反応ノート

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