反应 #1951055

反应方程式

1-Benzyl-4-phenyl-[1,4]azaphosphinane 4-oxide

HCl

→

4-phenyl-[1,4]azaphosphinane 4-oxide hydrochloride

溶剂

EtOH

反应条件

后处理

1. 1
   过滤After filtration through Celite
2. 2
   其他the residue was triturated with ether

实验过程

1-Benzyl-4-phenyl-[1,4]azaphosphinane 4-oxide (14.2 g, 49.8 mmol) was dissolved in absolute EtOH (65 mL) and 1N HCl (50 mL). Palladium on carbon (10%, 2.0 g) was added and the mixture was hydrogenated on a Parr shaker at 50 psi for 60 hours. After filtration through Celite, the filtrate was rotovapped and the residue was triturated with ether to give 4-phenyl-[1,4]azaphosphinane 4-oxide hydrochloride, as an off-white solid (11.40 g, 99%). 1H NMR (400 MHz, DMSO-d6) δ 7.85 (m, 2H), 7.65 (m, 3H), 3.5 (m, 4H), 2.7 (m, 2H), 2.2 (broad t, 2H). 31P NMR (DMSO-d6); δ 24.0 (s).

来源