Sodium Hydroxide → 4-(3-(2,6-Dimethylbenzyloxy)phenyl)butyric acid

HRID 516833ノート

反応式

HRID 516833 の反応式
[CH3:1][C:2]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][CH2:13][CH2:14][C:15]([O:17]CC)=[O:16])[CH:9]=[CH:10][CH:11]=1.[OH-].[Na+]>C(O)C>[CH3:1][C:2]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][CH2:13][CH2:14][C:15]([OH:17])=[O:16])[CH:9]=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 66875682Ethyl 4-(3-(2,6-dimethylbenzyloxy)phenyl)butanoate

生成物 1

HCID 219645274-(3-(2,6-Dimethylbenzyloxy)phenyl)butyric acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of Ethyl 4-(3-(2,6-dimethylbenzyloxy)phenyl)butanoate (Step B, 3.26 g, 10 mmol) in abs ethanol (60 ml) was treated with 1N NaOH (20 ml) at room temperature. The reaction mixture was stirred for 3 hours, or until all the starting material is gone, concentrated and diluted with chloroform and acidified by 1M HCl to bring the pH to 3.5-4. The organic layer was washed with brine, dried over Na2SO4, filtered, concentrated and purified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid) to give the title compound as white solid.

後処理

  1. concentrationconcentrated
  2. additiondiluted with chloroform
  3. washThe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by flash chromatography on a silica gel column (chloroform:methanol, 95:5 spiked with acetic acid)

出典と根拠

ORDレコード
ord-e8d3091c8d1a4b4ca9ff2806576b3bd7
出典データセット
uspto-grants-2015_08
特許番号
US09115072B2

反応ノート

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