HRID1592364
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added
- filtrationby filtering off the catalyst under N2 through a fiberglass
- filtrationfilter paper and vacuum
- customto obtain an oily residue which
- washwashed 2 times with 1N NaOH, 1 time with brine
- dry with materialdried (Na2SO4)