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

HRID 987244ノート

反応式

HRID 987244 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-927f498c4fb14148ba8935b4c7765e73
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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