2,2,6-Trimethyl-4H-1,3-dioxin-4-one → 3-(3-Acetoacetoxypropyl)-5-(4-chlorophenyl)-1-(4-methoxyphenyl) pyrazole
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=3)[N:11]=[C:10]([CH2:21][CH2:22][CH2:23][OH:24])[CH:9]=2)=[CH:4][CH:3]=1.[CH3:25][C:26]1[O:32]C(C)(C)O[C:28](=[O:29])[CH:27]=1>>[C:28]([O:24][CH2:23][CH2:22][CH2:21][C:10]1[CH:9]=[C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[N:12]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)[N:11]=1)(=[O:29])[CH2:27][C:26]([CH3:25])=[O:32]参加物
3
実験手順
5-(4-Chlorophenyl)-3-(3-hydroxypropyl)-1-(4-methoxyphenyl)pyrazole (1.71 g, 0.005 moles) and 2,2,6-trimethyl-1,3-dioxen-4-one (0.71 g, 0.005 moles) were disolved in 100 ml of xylenes. The solution was stirred under reflux for 16 hours. At that time, the solution was cooled to room temperature, and concentrated in vacuo to a yellow oil. The oil was flash chromatographed on silica gel to afford 59 (1.7 g, 80%) as a pale yellow oil.
後処理
- temperatureunder reflux for 16 hours
- concentrationconcentrated in vacuo to a yellow oil