反应 #40358

反应方程式

Boc-D-Phe-D-Phe-D-Leu-OBn

→

Boc-D-Phe-D-Phe-D-Leu-OH

溶剂

methanol

反应条件

后处理

1. 1
   其他In a flask flushed with nitrogen
2. 2
   workup.ADDITIONwas added wet palladium on carbon (1.8 g)
3. 3
   过滤After filtration through celite, methanol
4. 4
   其他was evaporated under reduced pressure
5. 5
   workup.DISSOLUTIONThe residue was dissolved in acetone (20 mL)
6. 6
   workup.ADDITIONslowly added to 500 mL water with 25 mL of 1N HCl under vigorous stirring

实验过程

In a flask flushed with nitrogen was added wet palladium on carbon (1.8 g) and a solution of Boc-D-Phe-D-Phe-D-Leu-OBn, intermediate 1-5 (11.1 g, 18.05 mmol) in methanol (50 μL). The mixture was stirred under a hydrogen balloon overnight. After filtration through celite, methanol was evaporated under reduced pressure. The residue was dissolved in acetone (20 mL) and slowly added to 500 mL water with 25 mL of 1N HCl under vigorous stirring. Pure product Boc-D-Phe-D-Phe-D-Leu-OH, intermediate 1-6 was obtained by filtration 9.4 g (99%). LC-MS: m/z=526 (M+H).

来源