Methylamine → 5-Methyl-2-nitro-4,5-dihydropyrazolo[1,5-a]pyrazin-6(7H)-one
反応式
Cl[CH2:2][C:3]1[N:7]([CH2:8][C:9]([O:11]CC)=O)[N:6]=[C:5]([N+:14]([O-:16])=[O:15])[CH:4]=1.[CH3:17][NH2:18]>ClCCl.O>[CH3:17][N:18]1[C:9](=[O:11])[CH2:8][N:7]2[N:6]=[C:5]([N+:14]([O-:16])=[O:15])[CH:4]=[C:3]2[CH2:2]1参加物
5
実験手順
To a solution of 146b (1.0 g, 4.0 mmol) in dichloromethane (30 mL) was added a solution of CH3NH2 (1.07 g, 12.0 mmol, 35% in methanol). This reaction mixture was stirred at room temperature for 3 h and diluted with water (30 mL). The organic layer was separated, dried over Na2SO4, and concentrated under reduced pressure. The residual was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 146c (450 mg, 57%) as a yellow solid. MS-ESI: [M+H]+ 196.9
後処理
- customThe organic layer was separated
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customThe residual was purified by silica-gel column chromatography
- washeluting with 30:1 dichloromethane/methanol
出典と根拠
- ORDレコード
- ord-0eddaca8ce3245a5b89ec99e63e3f91f
- 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…