Cesium carbonate → 1-(5-(Hydroxymethyl)-3-nitro-1H-pyrazol-1-yl)-2-methylpropan-2-ol
反応式
[N+:1]([C:4]1[CH:8]=[C:7]([CH2:9][OH:10])[NH:6][N:5]=1)([O-:3])=[O:2].C([O-])([O-])=O.[Cs+].[Cs+].[CH3:17][C:18]1([CH3:21])[CH2:20][O:19]1>>[OH:10][CH2:9][C:7]1[N:6]([CH2:17][C:18]([CH3:21])([OH:19])[CH3:20])[N:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:8]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
A sealed tube was charged with 139a (2.145 g, 15 mmol), Cs2CO3 (978 mg, 3.0 mmol), and 2,2-dimethyloxirane (15 mL). The mixture was stirred at 70° C. for 3 h. After cooled to room temperature, the mixture was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with petroleum ether/ethyl acetate (5:1 to 1:1) to afford 139b (1.2 g, 38%) as a white solid. MS-ESI: [M+H]+ 216.2
後処理
- temperatureAfter cooled to room temperature
- concentrationthe mixture was concentrated under reduced pressure
- customThe residue was purified by silica-gel column chromatography
- washeluting with petroleum ether/ethyl acetate (5:1 to 1:1)
出典と根拠
- ORDレコード
- ord-dce15c824df7468bbda5d444733c1cb0
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08669251B2
反応ノート
読み込み中…