Allylamine → Ammonium Hydroxide
反応式
[CH:1]1([CH:4]=[O:5])[CH2:3][CH2:2]1.[CH2:6]([NH2:9])[CH:7]=[CH2:8].C([BH3-])#N.[Na+]>CO>[NH4+:9].[OH-:5].[CH:1]1([CH2:4][NH:9][CH2:6][CH:7]=[CH2:8])[CH2:3][CH2:2]1参加物
6
実験手順
Cyclopropanecarboxaldehyde (1.00 g, 14.3 mmol) was added dropwise to a stirred solution of allylamine (4.07 g, 71.3 mmol) in MeOH (100 mL) and stirring was continued at ambient temperature for 2 h, then sodium cyanoborohydride (0.94 g, 15.0 mmol) was added. After 3 h, the solvent was removed under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of CH2Cl2:MeOH:NH4OH—100:0:0 to 90:10:1 to provide the title compound as a yellow oil. MS: m/z=112 (M+1).
後処理
- waitAfter 3 h
- customthe solvent was removed under reduced pressure
- customThe crude product was purified by silica gel chromatography
- washeluting with a gradient of CH2Cl2
出典と根拠
- ORDレコード
- ord-36d995fe03094da68f0ee8534ba26c18
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07192954B2
反応ノート
読み込み中…