Potassium Carbonate → Benzene, 1-chloro-4-ethynyl-
反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]#[C:15][Si](C)(C)C)=[CH:10][CH:9]=1>CO>[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]#[CH:15])=[CH:10][CH:9]=1参加物
4
実験手順
Anhydrous potassium carbonate (0.9g, 0.0065 moles) was added to a solution of chloro-4-trimethylsilylethynylbenzene (3.Og, 0.014 moles) in methanol (60 cm3) under an atmosphere of nitrogen. The reaction was stirred, under nitrogen, at room temperature for 4 hours. The solvent was removed, the solid residue was tritura&ed with ether and then dichloromethane and filtered. The organic filtrates were combined and evaporated to dryness giving chloro-4-ethynylbenzene as a brown solid. This was used in the next step without any further purification yield 1.1 g (58%). 1H NMR 67.3 (2H, d), 7.4 (2H, d), 3.1 (1H, s)ppm.
後処理
- customThe solvent was removed
- filtrationdichloromethane and filtered
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-b2dde32b2daa4aa9a7ad714a99242910
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05208239
反応ノート
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