Potassium Carbonate → Ethyl 3-ethynylbenzoate

HRID 1760088노트

반응식

HRID 1760088 반응식
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[CH:14]=[C:15]([CH:21]=[CH:22][CH:23]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17])(C)C>C(O)C>[C:12]([C:13]1[CH:14]=[C:15]([CH:21]=[CH:22][CH:23]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17])#[CH:11]

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 22600505Ethyl 3-((trimethylsilyl)ethynyl)benzoate

생성물 1

HCID 15540684Ethyl 3-ethynylbenzoate수율 96%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Potassium carbonate (583 mg, 4.22 mmol) was added to an ethanol solution (10 ml) of ethyl 3-[(trimethylsilyl)ethynyl]benzoate (1.04 g, 4.22 mmol), and stirred at room temperature for 2 h. The mixture was concentrated, and the residue was dissolved in ethyl acetate. The organic layer was washed with water and then brine, dried over sodium sulfate and concentrated. The residue was purified by silica gel flash column chromatography (eluent: hexane/ethyl acetate=30/1) to give ethyl 3-ethynylbenzoate (96%).

후처리

  1. concentrationThe mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialbrine, dried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel flash column chromatography (eluent: hexane/ethyl acetate=30/1)

출처 및 근거

ORD 기록
ord-2ae273aae2844941bfd776dcc30f0715
출처 데이터셋
uspto-grants-2005_01
특허 번호
US06838574B1

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