Potassium Carbonate → Ethyl 3-ethynylbenzoate

HRID 1760088ノート

反応式

HRID 1760088 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 15540684Ethyl 3-ethynylbenzoate収率 96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-2ae273aae2844941bfd776dcc30f0715
出典データセット
uspto-grants-2005_01
特許番号
US06838574B1

反応ノート

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