HRID1592364

反应详情

EQUATION

反应方程式

HRID 1592364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Pd(OH)2 was carefully wetted down under N2 with 10 mL of MeOH then the product of Step f (1.15 g) dissolved in 40 mL of MeOH was added followed by 50 mL of HOAc. The mixture was hydrogenated overnight on a Parr shaker at 50 PSI. Worked up by filtering off the catalyst under N2 through a fiberglass filter paper and vacuum. The filtrate was stripped to obtain an oily residue which was dissolved in 25 mL of Et2O and washed 2 times with 1N NaOH, 1 time with brine, dried (Na2SO4) and stripped to give 0.57 g of a light yellow oil. MS (ESI) detects (M+H)+=255.

WORKUP

后处理

  1. additionwas added
  2. filtrationby filtering off the catalyst under N2 through a fiberglass
  3. filtrationfilter paper and vacuum
  4. customto obtain an oily residue which
  5. washwashed 2 times with 1N NaOH, 1 time with brine
  6. dry with materialdried (Na2SO4)