Sodium hydride → HCID 178526672、化合物
反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][N:11]=[C:12]([C:19]([F:22])([F:21])[F:20])[CH2:13][C:14](OCC)=[O:15])=[CH:6][CH:5]=1)([O-:3])=[O:2].[H-].[Na+]>C1COCC1>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[C:14]([OH:15])=[CH:13][C:12]([C:19]([F:22])([F:21])[F:20])=[N:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]参加物
4
反応条件
- 温度
- 50 °C
実験手順
To a mixture of 382 mg (1.2 mmol) of ethyl trifluoroacetoacetate 4-nitrophenylhydrazone in 10 ml of THF was added 53 mg (60%; 1.32 mmol) of NaH and the resulting mixture was stirred at room temperature for 4 hours and at 50° C. for 16 hours. The reaction mixture was quenched with ammonium chloride solution, the aqueous layer was extracted with ethyl acetate (3×), and the combined organic layer was dried and concentrated in vacuo. The residue was purified by column chromatography (silica gel; 50% ethyl acetate in hexane) and recrystallized from methylene chloride/hexane to afford 1-(4-nitrophenyl)-3-trifluoromethyl-5-hydroxypyrazole as a white solid.