Hydrochloric Acid → 1-{(2-Ethoxycarbonylethyl)-[4-(4-fluorophenoxy)benzenesulfonyl]-amino}-cyclopentanecarboxylic Acid

HRID 1976906노트

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HRID 1976906 반응식
C1([NH2+]C2CCCCC2)CCCCC1.[CH2:14]([O:16][C:17]([CH2:19][CH2:20][N:21]([S:30]([C:33]1[CH:38]=[CH:37][C:36]([O:39][C:40]2[CH:45]=[CH:44][C:43]([F:46])=[CH:42][CH:41]=2)=[CH:35][CH:34]=1)(=[O:32])=[O:31])[C:22]1([C:27]([O-:29])=[O:28])[CH2:26][CH2:25][CH2:24][CH2:23]1)=[O:18])[CH3:15].Cl>ClCCl>[CH2:14]([O:16][C:17]([CH2:19][CH2:20][N:21]([S:30]([C:33]1[CH:34]=[CH:35][C:36]([O:39][C:40]2[CH:41]=[CH:42][C:43]([F:46])=[CH:44][CH:45]=2)=[CH:37][CH:38]=1)(=[O:32])=[O:31])[C:22]1([C:27]([OH:29])=[O:28])[CH2:26][CH2:25][CH2:24][CH2:23]1)=[O:18])[CH3:15]

참가 물질

4

실험 절차

A solution of 3.0 g (4.5 mmol) of 1-{(2-ethoxycarbonylethyl)-[4-(4-fluorophenoxy)benzenesulfonyl]amino}cyclopentanecarboxylic acid, dicyclohexylaminium salt in 30 mL of dichloromethane was treated with 30 mL of 2N hydrochloric acid at ambient temperature causing immediate precipitation of solids. This mixture was stirred at ambient temperature for three hours. The solids were filtered, the aqueous phase was extracted with dichloromethane, and the combined organic phases were washed with water, dried over sodium sulfate, and concentrated under vacuum to 2.2 g (100%) of 1-{(2-ethoxycarbonylethyl)-[4-(4-fluorophenoxy)benzenesulfonyl]amino}cyclopentanecarboxylic acid as a clear oil.

후처리

  1. customprecipitation of solids
  2. filtrationThe solids were filtered
  3. extractionthe aqueous phase was extracted with dichloromethane
  4. washthe combined organic phases were washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under vacuum to 2.2 g (100%) of 1-{(2-ethoxycarbonylethyl)-[4-(4-fluorophenoxy)benzenesulfonyl]amino}cyclopentanecarboxylic acid as a clear oil

출처 및 근거

ORD 기록
ord-58503d7180fb415f9359ec76a713ebef
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06229025B1

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