HRID1763148

反应详情

EQUATION

反应方程式

HRID 1763148 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2.5 g (0.0059 mol) of product of Example 81, 0.6 g (0.0059 mol) of triethylamine and 0.25 g of 5% Pd/C (50% water coated) in 100 ml of ethanol was hydrogenated (446 kPa, for 18 hours at 50° C. The mixture was then filtered through celite and concentrated in vacuo to remove the ethyl alcohol. The residue was poured into water, and extracted with diethyl ether. The ether extract was washed with water, then dried over MgSO4. The dry ether phase was then concentrated in vacuo to yield 2.00 g of a yellow solid. This solid was then recrystallized in hexane to yield 1.28 g (56%) of product as a tan solid; mp 61° C.

WORKUP

后处理

  1. filtrationThe mixture was then filtered through celite and
  2. concentrationconcentrated in vacuo
  3. customto remove the ethyl alcohol
  4. additionThe residue was poured into water
  5. extractionextracted with diethyl ether
  6. extractionThe ether extract
  7. washwas washed with water
  8. dry with materialdried over MgSO4
  9. concentrationThe dry ether phase was then concentrated in vacuo