Tetrahydrofuran → HCID 15614953、化合物
反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:16][CH3:17])[C:8]=2[C:12]([F:15])([F:14])[F:13])[C:3]=1C(O)=O.[CH2:21]([O:23][C:24]([N:26]=[C:27]=NC(C)(C)C)=[O:25])[CH3:22].[O:33]1CCCC1>>[Cl:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:16][CH3:17])[C:8]=2[C:12]([F:15])([F:13])[F:14])[C:3]=1[C:27]([NH:26][C:24](=[O:25])[O:23][CH2:21][CH3:22])=[O:33]参加物
4
実験手順
A solution of 2-chloro-6-methoxy-5-(trifluoromethyl)naphthoic acid (3.50 g, 11.5 mmol, prepared by the process of Example 14), and ethoxycarbonyl-t-butylcarbodiimide (2.2 g, 1.1 eq) in dry tetrahydrofuran (58 mL) was heated to reflux under a dry nitrogen atmosphere for 51/2 hours. The tetrahydrofuran was removed and the resultant solid was triturated with ether (2×15 mL) and dried in vacuo. A second crop was recovered from the ether and combined with the product (3.36 g, 78%). The small sample was further purified by flash chromatography (70/30 petroleum ether/ethyl acetate) to provide the analytically pure product as a white solid, m.p. 169°-171° C.