反応 #68414

反応方程式

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
   抽出extracted with EtOAc (×3)
5. 5
   洗浄The combined organic layer was washed with brine
6. 6
   乾燥dried over Na2SO4
7. 7
   濃縮concentrated in vacuo
8. 8
   workup.DISTILLATIONThe crude product was purified by distillation under vacuum

実験手順

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.

出典