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Sodium Hydroxide → 2-(3-(4-(Trifluoromethyl)benzyloxy)phenyl)acetic acid

HRID 516830
ノート
印刷プレビュー

反応式

HRID 516830 の反応式
[F:1][C:2]([F:24])([F:23])[C:3]1[CH:22]=[CH:21][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]([CH2:15][C:16]([O:18]CC)=[O:17])[CH:12]=[CH:13][CH:14]=2)=[CH:5][CH:4]=1.[OH-].[Na+]>C(O)C>[F:1][C:2]([F:23])([F:24])[C:3]1[CH:4]=[CH:5][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]([CH2:15][C:16]([OH:18])=[O:17])[CH:12]=[CH:13][CH:14]=2)=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 11974618Ethyl 2-(3-(4-(trifluoromethyl)benzyloxy)phenyl)acetate

生成物 1

HCID 119749282-(3-(4-(Trifluoromethyl)benzyloxy)phenyl)acetic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution Ethyl 2-(3-(4-(trifluoromethyl)benzyloxy)phenyl)acetate (Step A, 6 g, 17.7 mmol) in absolute ethanol (70 ml) was added 1N NaOH (36 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-711b903c44ee4b4e9b52ced45e490068
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115072B2

反応ノート

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