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

HRID 987253노트

반응식

HRID 987253 반응식
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]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 824082-Propanesulfonyl chlorideHCID 54239207HCID 54239207, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4fdfdc209e8c45d3a1980db436027294
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630600B1

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