Potassium Carbonate → 2-Cyclopropyloxy-5-trifluoromethoxyphenylethyne

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[C:1](=O)([O-])[O-].[K+].[K+].[CH:7]1([O:10][C:11]2[CH:18]=[CH:17][C:16]([O:19][C:20]([F:23])([F:22])[F:21])=[CH:15][C:12]=2[CH:13]=O)[CH2:9][CH2:8]1.P(=O)(OC=[N+]=[N-])OC(=O)C>CO>[CH:7]1([O:10][C:11]2[CH:18]=[CH:17][C:16]([O:19][C:20]([F:23])([F:22])[F:21])=[CH:15][C:12]=2[C:13]#[CH:1])[CH2:9][CH2:8]1

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실험 절차

Potassium carbonate (6.15 g, 44 mmol) was added to a stirred solution of 2-cyclopropyloxy-5-trifluoromethoxybenzaldehyde (Description 3; 4.4 g, 17.8 mmol), and acetyl diazomethyl phosphonate (6.15 g, 32 mmol) in dry methanol (50 ml) at +5° C. The reaction mixture was stirred at +5° C. for 30 minutes and at room temperature for 3.5 hours. The mixture was quenched with saturated aqueous ammonium chloride and extracted into hexane (3×30 ml). The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (iso-hexane:diethyl ether 0-45%) to give the title compound (4.2 g, 94%).