Sodium borohydride → 1-(1-(2-Bromoethyl)-3-(2,5-dimethyl-1H-pyrrol-1-yl)-1H-pyrazol-5-yl)ethanol
反応式
[Br:1][CH2:2][CH2:3][N:4]1[C:8]([C:9](=[O:11])[CH3:10])=[CH:7][C:6]([N:12]2[C:16]([CH3:17])=[CH:15][CH:14]=[C:13]2[CH3:18])=[N:5]1.[BH4-].[Na+]>CO>[Br:1][CH2:2][CH2:3][N:4]1[C:8]([CH:9]([OH:11])[CH3:10])=[CH:7][C:6]([N:12]2[C:16]([CH3:17])=[CH:15][CH:14]=[C:13]2[CH3:18])=[N:5]1参加物
4
実験手順
A 100-mL round-bottomed flask equipped with a magnetic stirrer was charged with 150e (2.1 g, 1.0 eq., 6.8 mmol), NaBH4 (1.29 g, 5.0 eq., 34.0 mmol), and methanol (50 mL). The mixture was stirred at room temperature for 2 h and quenched with water (30 mL). It was then concentrated under reduced pressure and the residue was extracted with dichloromethane (3×50 mL). The combined organic layer was concentrated under reduced pressure to afford crude 150f, which was used in the next step without further purification. MS-ESI: [M+H]+ 311.9
後処理
- customA 100-mL round-bottomed flask equipped with a magnetic stirrer
- customquenched with water (30 mL)
- concentrationIt was then concentrated under reduced pressure
- extractionthe residue was extracted with dichloromethane (3×50 mL)
- concentrationThe combined organic layer was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-7f3c3d70b82949dea8c1dbfa08da8357
- 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…