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

HRID 516833노트

반응식

HRID 516833 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e8d3091c8d1a4b4ca9ff2806576b3bd7
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115072B2

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