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Potassium Carbonate → 2-(3-Ethynyl-phenyl)-2-methyl-propionic acid ethyl ester

HRID 2377457
ノート
印刷プレビュー

反応式

HRID 2377457 の反応式
[CH2:1]([O:3][C:4](=[O:20])[C:5]([CH3:19])([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]#[C:14][Si](C)(C)C)[CH:8]=1)[CH3:6])[CH3:2].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:1]([O:3][C:4](=[O:20])[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]#[CH:14])[CH:8]=1)([CH3:6])[CH3:19])[CH3:2]
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 11430Potassium CarbonateHCID 57424257HCID 57424257、化合物2 回

生成物 1

HCID 574242582-(3-Ethynyl-phenyl)-2-methyl-propionic acid ethyl ester収率 72.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-methyl-2-(3-trimethylsilanylethynyl-phenyl)-propionic acid ethyl ester (Intermediate 131, 0.74 g, 2.56 mmol) in ethanol (10 mL) was treated with potassium carbonate (0.2 g, 1.45 mmol). The resulting reaction mixture was stirred at ambient temperature overnight. The volatiles were evaporated in vacuo and the residue was diluted with water and extracted with diethyl ether. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to a residue that was subjected to flash column chromatography over silica gel (230-400 mesh) using 1-5% ethyl acetate in hexane as the eluent to afford the title product (0.4 g, 72%).

後処理

  1. customThe resulting reaction mixture
  2. customThe volatiles were evaporated in vacuo
  3. additionthe residue was diluted with water
  4. extractionextracted with diethyl ether
  5. washThe organic phase was washed with water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo to a residue that

出典と根拠

ORDレコード
ord-4bb0ade053474eb8b86f879121fdda33
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07468391B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート