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

HRID 987238ノート

反応式

HRID 987238 の反応式
O.[OH-].[Li+].C([O:6][C:7](=[O:34])[CH:8]([O:31][CH2:32][CH3:33])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][S:27]([CH3:30])(=[O:29])=[O:28])=[CH:22][CH:21]=2)[CH:11]=1)C>O.O1CCCC1>[CH2:32]([O:31][CH:8]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH2:17][CH2:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]([O:26][S:27]([CH3:30])(=[O:28])=[O:29])=[CH:24][CH:25]=2)[CH:11]=1)[C:7]([OH:34])=[O:6])[CH3:33]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 22988419Ethyl 2-ethoxy-3-{3-[3-(4-methylsulfonyloxyphenyl)propoxy]phenyl}propanoate

生成物 1

HCID 229887272-Ethoxy-3-[3-(3-{4-methanesulfonyloxyphenyl}propoxy)phenyl]propanoic acid収率 109.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Lithium hydroxide hydrate (91.1 mg; 2.7 mmole) in water (6.6 ml) was slowly added to a solution of 2-ethoxy-3-{3-[3-(4-methanesulfonyloxyphenyl)propoxy]phenyl}propanoic acid ethyl ester (described in Example 12d) (0.889 g; 1.97 mmole) in tetrahydrofuran (9 ml). After stirring at room temperature for 5 hours tetrahydrofuran was removed by evaporation in vacuo. The residue was washed with diethyl ether and ethyl acetate. The water phase was acidified with potassium hydrogen sulfate (1M), and extracted with ethyl acetate and dichloromethane. The organic phases were combined, dried (sodium sulfate), filtered and the solvent was evaporated in vacuo to give 0.91 g of 2-ethoxy-3-[3-(3-{4-methanesulfonyloxyphenyl}propoxy)phenyl]propanoic acid.

後処理

  1. customwas removed by evaporation in vacuo
  2. washThe residue was washed with diethyl ether and ethyl acetate
  3. extractionextracted with ethyl acetate and dichloromethane
  4. dry with materialdried (sodium sulfate)
  5. filtrationfiltered
  6. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-a940f089e2d942d4aee45e6d96ccafd5
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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