HRID333656

反应详情

EQUATION

反应方程式

HRID 333656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The compound (1.0 eq.) obtained in Step 1 was dissolved in a mixed solvent of ethylalcohol/methylene chloride (3:1, 0.01˜0.1 M) to which Pd(OH)2 (500 massa) was then added. The resulting reaction mixture was stirred for 5˜8 hrs at room temperature under 1 atm of hydrogen gas. After the filtration of the metal catalyst through a Celite pad, the reaction mixture was washed with a solution of ethylalcohol/methylene:chloride (3:1). After two rounds of centrifugation at 1000 rpm for 10 min, the supernatant was concentrated and dried in a vacuum. The concentrate was precipitated in a mixed solvent of hexane/ethyl acetate (1:1) to afford the object compound as a white wax solid (24 mg, 80%).

WORKUP

后处理

  1. additionwas then added
  2. customThe resulting reaction mixture
  3. filtrationAfter the filtration of the metal catalyst through a Celite pad
  4. washthe reaction mixture was washed with a solution of ethylalcohol/methylene
  5. concentrationthe supernatant was concentrated
  6. customdried in a vacuum
  7. customThe concentrate was precipitated in a mixed solvent of hexane/ethyl acetate (1:1)