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

HRID 987244노트

반응식

HRID 987244 반응식
O.[OH-].[Li+].C[O:5][C:6](=[O:36])[CH:7]([O:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][S:25]([CH3:28])(=[O:27])=[O:26])=[CH:20][CH:19]=2)=[CH:11][CH:10]=1>O.O1CCCC1>[CH2:30]([O:29][CH:7]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([O:24][S:25]([CH3:28])(=[O:27])=[O:26])=[CH:22][CH:23]=2)=[CH:11][CH:10]=1)[C:6]([OH:36])=[O:5])[CH2:31][CH2:32][CH2:33][CH2:34][CH3:35]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 569752562-Hexyloxy-3-[4-(2-{4-methanesulfonyloxyphenyl}-ethoxy)phenyl]propanoic acid methyl ester

생성물 1

HCID 229886862-Hexyloxy-3-[4-(2-{4-methanesulfonyloxyphenyl}-ethoxy)phenyl]propanoic acid수율 97.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide hydrate (0.036 g; 0.85 mmole) dissolved in water (2.6 ml) was slowly added at room temperature to a solution of 2-hexyloxy-3-[4-(2-{4-methanesulfonyloxyphenyl}ethoxy)phenyl]propanoic acid methyl ester (described in Example 16) (0.37 g; 0.77 mmole) in tetrahydrofuran (3.5 ml). The reaction mixture was stirred at room temperature for 3.5 hours and then evaporated to remove tetrahydrofuran. The residue was acidified with potassium hydrogen sulfate (1 M) until pH<2 and then extracted with ethyl acetate. The organic phase was washed with brine and dried. Evaporation to remove the solvent gave 0.349 g (97.5%) of 2-hexyloxy-3-[4-(2-{4-methanesulfonyloxyphenyl}-ethoxy)phenyl]propanoic acid.

후처리

  1. customevaporated
  2. customto remove tetrahydrofuran
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with brine
  5. customdried
  6. customEvaporation
  7. customto remove the solvent

출처 및 근거

ORD 기록
ord-927f498c4fb14148ba8935b4c7765e73
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630600B1

반응 노트

불러오는 중…