Methanol → Methyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylate
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]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([OH:23])=[O:22])[C:9]=2[CH3:24])=[CH:4][CH:3]=1.[CH3:25]O>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([O:23][CH3:25])=[O:22])[C:9]=2[CH3:24])=[CH:6][CH:7]=1参加物
3
実験手順
19.54 g of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid are dissolved in 350 ml of MeOH, 0.97 g of paratoluenesulfonic acid is added and the mixture is then refluxed for 18 hours. After evaporation of the solvent, the residue is taken up with AcOEt and washed with saturated NaHCO3 solution and then with saturated NaCl solution. It is dried over MgSO4, the insoluble material is filtered off and the filtrate is then concentrated to dryness to give 18.53 g of the expected compound, m.p.=133° C.
後処理
- temperaturethe mixture is then refluxed for 18 hours
- customAfter evaporation of the solvent
- washwashed with saturated NaHCO3 solution
- dry with materialIt is dried over MgSO4
- filtrationthe insoluble material is filtered off
- concentrationthe filtrate is then concentrated to dryness
出典と根拠
- ORDレコード
- ord-5d15404827ee44daa2120a4c7c345c9c
- 出典データセット
- uspto-grants-2000_02
- 特許番号
- US06028084
反応ノート
読み込み中…