反应 #1951053

反应方程式

HCl

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

→

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

溶剂

ethanol

反应条件

后处理

1. 1
   过滤The mixture was filtered through Celite
2. 2
   其他all solvents were removed under reduced pressure
3. 3
   其他The product was triturated in hot ethanol (50 mL)
4. 4
   温度cooled
5. 5
   workup.ADDITIONthe solution was diluted with ether (300 mL)
6. 6
   过滤The white crystalline solid was filtered
7. 7
   洗涤washed with ether (2×50 mL), hexane (2×50 mL)
8. 8
   其他dried in vacuo

实验过程

1-Benzyl-4-methyl-[1,4]azaphosphinane 4-oxide was dissolved in ethanol (100 mL). 1 M HCl (100 mL) was added, along with palladium on carbon (10%, 2.6 g). The mixture was hydrogenated on a Parr shaker for 4 hours at 50 psi. The mixture was filtered through Celite and all solvents were removed under reduced pressure. The product was triturated in hot ethanol (50 mL) and cooled, and the solution was diluted with ether (300 mL). The white crystalline solid was filtered, washed with ether (2×50 mL), hexane (2×50 mL), and dried in vacuo. 4-methyl-[1,4]azaphosphinane 4-oxide hydrochloride was obtained as a white crystalline solid (9.46 g, 94%). 1H NMR (400 MHz, DMSO) δ 3.07 (m, 2H); 2.68 (m, 2H); 1.78 (m, 2H); 1.61 (m, 2H), 1.39 (3H, d, JH-C-P=13.6 Hz.); 31P NMR: δ 29 ppm; ESMS (m/z): (M+1)+ found, 134.

来源