HRID42536

反应详情

EQUATION

反应方程式

HRID 42536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10% Pd/C (Degussa, 50% wet, 1.0 g, 9.40 mmol) was carefully wetted down under argon with ethanol, and then (7S,8R)-ethyl 8-((R)-1-phenylethylamino)-1,4-dioxaspiro[4.5]decane-7-carboxylate p-toluenesulfonic acid salt (10.3 g, 20.37 mmol) in ethanol (75 mL) was added. The mixture was then hydrogenated on a Parr Shaker apparatus for about 16 hours at 50 psi. Under argon, the reaction was carefully filtered through a fiberglass filter paper. The filtrate was concentrated to give (7S,8R)-ethyl 8-amino-1,4-dioxaspiro[4.5]decane-7-carboxylate p-toluenesulfonic acid salt (8.10 g, 20.18 mmol, 99% yield) as a tacky white glass. MS (ESI+)=230.12 (M+H)+.

WORKUP

后处理

  1. filtrationUnder argon, the reaction was carefully filtered through a fiberglass
  2. filtrationfilter paper
  3. concentrationThe filtrate was concentrated