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Water → 2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid

HRID 61814
ノート
印刷プレビュー

反応式

HRID 61814 の反応式
C([O:3][C:4](=[O:20])[C:5]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH:15]([CH3:17])[CH3:16])=[C:10]([O:18][CH3:19])[CH:9]=1)([CH3:7])[CH3:6])C.[OH-].[Na+].O>C1COCC1.CCO>[CH:15]([O:14][C:11]1[CH:12]=[CH:13][C:8]([C:5]([CH3:7])([CH3:6])[C:4]([OH:20])=[O:3])=[CH:9][C:10]=1[O:18][CH3:19])([CH3:16])[CH3:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 66834644HCID 66834644、化合物

生成物 1

HCID 668346712-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid ethyl ester (Compound L3-1, 1.45 g, 5.17 mmol) was dissolved in THF (13 mL) and EtOH (13 mL), added with 1 N aqueous solution of sodium hydroxide (10.3 mL, 2.0 eq.), and stirred at 80° C. overnight. The reaction solution was added to water and extracted with ethyl acetate. The aqueous layer was acidified by using 1 N aqueous solution of hydrochloric acid, extracted with ethyl acetate, washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white solid, 1.10 g, 84%).

後処理

  1. extractionextracted with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. customThe drying agent was removed by filtration
  6. customthe residues obtained
  7. concentrationafter concentration under reduced pressure
  8. customwere purified by silica gel column chromatography (ethyl acetate/hexane)
  9. customto obtain the target compound (white solid, 1.10 g, 84%)

出典と根拠

ORDレコード
ord-f865c7d0fe7f44da81d69c156db8f76c
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440922B2

反応ノート

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