反応 #68413

反応方程式

HCl

2,6-dichloro-5-fluoronicotinonitrile

→

title compound

(2,6-Dichloro-5-fluoropyridin-3-yl)methanamine

溶媒

MeOH

反応条件

後処理

1. 1
   その他To a Parr reaction bottle
2. 2
   ろ過filtered
3. 3
   濃縮concentrated
4. 4
   workup.DISSOLUTIONThe crude was dissolved in EtOAc
5. 5
   その他the layers were separated
6. 6
   洗浄The organic layer was washed with brine
7. 7
   乾燥dried over Na2SO4
8. 8
   濃縮concentrated in vacuo

実験手順

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 6 M HCl (50 ml) and a solution of 2,6-dichloro-5-fluoronicotinonitrile (Aldrich, 10.0 g, 52.4 mmol) in MeOH (100 ml). The mixture was placed under 50 psi H2 on a shaker type Parr apparatus for 21 h, filtered and concentrated. The crude was dissolved in EtOAc, basified with aqueous NaOH, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as crude light yellow oil. Used without further purification.

出典