反应 #68414

反应方程式

NH3.H2O

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

Compound 144

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

→

title compound

(5-Fluoropyridin-3-yl)methanamine

溶剂

MeOH

反应条件

后处理

1. 1
   其他To a Parr reaction bottle
2. 2
   过滤filtered
3. 3
   浓缩concentrated
4. 4
   萃取extracted with EtOAc (×3)
5. 5
   洗涤The combined organic layer was washed with brine
6. 6
   干燥dried over Na2SO4
7. 7
   浓缩concentrated in vacuo
8. 8
   workup.DISTILLATIONThe crude product was purified by distillation under vacuum

实验过程

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 28% NH3.H2O (50 ml) and a solution of (2,6-dichloro-5-fluoropyridin-3-yl)methanamine (Compound 144, 10.1 g, 52 mmol) in MeOH (100 ml). The mixture was placed under 51 psi H2 on a shaker type Parr apparatus for 16 h, filtered and concentrated. The resulting aqueous solution was basified with NaOH, extracted with EtOAc (×3). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by distillation under vacuum to yield the title compound as colorless oil.

来源