Lithium hydroxide, monohydrate → 2-Ethoxy-3-{4-[2-(4-methanesulfonylaminophenyl)ethoxy]phenyl}propanoic acid

HRID 987307노트

반응식

HRID 987307 반응식
C([O:3][C:4](=[O:30])[CH:5]([O:27][CH2:28][CH3:29])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([NH:22][S:23]([CH3:26])(=[O:25])=[O:24])=[CH:18][CH:17]=2)=[CH:9][CH:8]=1)C.O.[OH-].[Li+]>O1CCCC1.O>[CH2:28]([O:27][CH:5]([CH2:6][C:7]1[CH:8]=[CH:9][C:10]([O:13][CH2:14][CH2:15][C:16]2[CH:17]=[CH:18][C:19]([NH:22][S:23]([CH3:26])(=[O:24])=[O:25])=[CH:20][CH:21]=2)=[CH:11][CH:12]=1)[C:4]([OH:30])=[O:3])[CH3:29]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 54054669HCID 54054669, 화합물

생성물 1

HCID 99093362-Ethoxy-3-{4-[2-(4-methanesulfonylaminophenyl)ethoxy]phenyl}propanoic acid수율 104.3%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

2-Ethoxy-3-{4-[2-(4-methanesulfonylaminophenyl)ethoxy]phenyl}propanoic acid ethyl ester (described in Example 62) (0.554 g; 1.27 mmole) was dissolved in tetrahydrofuran (5.7 ml). Lithium hydroxide hydrate (0.137 g; 3,26 mmole) was dissolved in water and added in portions during 30 minutes at room temperature. The reaction mixture was kept in the refrigerator over night. Tetrahydrofuran was evaporated in vacuo. The water residue was washed with ethyl acetate, acidified with hydrochloric acid (1M) to pH 1-2 and the mixture was extracted with ethyl acetate. The organic phase was washed with brine, dried (sodium sulfate), filtered and the solvent was evaporated in vacuo to give 0.54 g (yield 100%) of 2-ethoxy-3-{4-[2-(4-methanesulfonylaminophenyl)ethoxy]phenyl}propanoic acid.

후처리

  1. additionadded in portions during 30 minutes at room temperature
  2. waitThe reaction mixture was kept in the refrigerator over night
  3. customTetrahydrofuran was evaporated in vacuo
  4. washThe water residue was washed with ethyl acetate
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic phase was washed with brine
  7. dry with materialdried (sodium sulfate)
  8. filtrationfiltered
  9. customthe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-ab31c29587194e13942254b04e423e96
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630600B1

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