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

HRID 1765844
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HRID 1765844 반응식
[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]
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 57424257HCID 57424257, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e9bd5776bd584bf78ec4530753b57e51
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07226951B2

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