反応式
[F:1][C:2]1[C:3]([C:9]#[N:10])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1.[ClH:11]>[Pd].C(O)C.O1CCCC1>[ClH:11].[F:1][C:2]1[C:3]([CH2:9][NH2:10])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1参加物
5
実験手順
A mixture of 3,5-difluoropicolinonitrile (1.4 g, 10 mmol), conc.HCl (12 ml) and 10% Pd—C (200 mg) in 1:1 ethanol/tetrahydrofuran was shaken under a hydrogen atmosphere (50 psi) for 5 h. The reaction mixture was filtered and the ethanol removed in vacuo. The remaining solution was lyophilized to afford an off-white solid (2.16 g, 100% yield). LCMS (M+H) calcd for C6H7F2N2: 145.06. found: 145.12.
後処理
- filtrationThe reaction mixture was filtered
- customthe ethanol removed in vacuo
出典と根拠
- ORDレコード
- ord-5a4e999dfdc745588a16416be98a9c54
- 出典データセット
- uspto-grants-2007_01
- 特許番号
- US07157447B2
関連ノート
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