Lithium Hydroxide → HCID 18443662、化合物

HRID 459148

反応式

HRID 459148 の反応式
[OH-].[Li+].C[O:4][C:5](=[O:19])[CH:6]([O:17][CH3:18])[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[C:10]([O:15][CH3:16])[CH:9]=1>C1COCC1>[OH:14][C:11]1[CH:12]=[CH:13][C:8]([CH2:7][CH:6]([O:17][CH3:18])[C:5]([OH:19])=[O:4])=[CH:9][C:10]=1[O:15][CH3:16]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 588230083-(4-Hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid methyl ester

生成物 1

HCID 18443662HCID 18443662、化合物収率 74%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A 1N aqueous lithium hydroxide solution was added to a solution of 3-(4-hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid methyl ester (280 mg, 1.17 mmol) in THF at room temperature, and the reaction mixture stirred overnight. The aqueous phase was extracted with ethyl acetate (20 mL), acidified to pH 2, and extracted with ethyl acetate (3×15 mL). The later organic layers were combined and washed with water (15 mL) and brine (10 mL), dried (MgSO4), filtered, and concentrated under vacuum to produce 3-(4-hydroxy-3-methoxy-phenyl)-2-methoxy-propionic acid as an oil (183 mg, 74%). 1H-NMR (250.13 MHz, CDCl3): δ 6.83 (1H, d, J=7.8), 6.74 (1H, s), 6.72 (1H, d, J=7.8), 3.99 (1H dd, J=7.8, 4.0), 3.85 (s, 3H), 3.40 (s, 3H), 3.09 (1H, dd, J=14.2, 4.0), 2.91 (1H dd, J=14.2, 7.8).

後処理

  1. extractionThe aqueous phase was extracted with ethyl acetate (20 mL)
  2. extractionextracted with ethyl acetate (3×15 mL)
  3. washwashed with water (15 mL) and brine (10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-2d4d67a8859f406389ddf0bfde39991c
出典データセット
uspto-grants-2007_03
特許番号
US07192982B2

関連ノート

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