HRID1859314

反应详情

EQUATION

反应方程式

HRID 1859314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methanol (60 ml) and 10% Pd/C (500 mg) were added to 4-[9-(t-butyl-dimethylsilyloxy)-1-nonynyl]-7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman (560 mg, 1.01 mmol) obtained in Example 28, and the mixture was stirred for 2 days under hydrogen gas (normal pressure). Ethyl acetate was added to the reaction solution which was then filtered, washed several times with ethyl acetate and concentrated under reduced pressure to remove the organic solvent. To the residue were added methanol (60 ml) and 10% Pd/C (300 mg), and the reaction mixture was stirred for 8 hours at 5 atomsphere under hydrogen gas. Ethyl acetate was added again to the reaction solution which was then filtered and concentrated under reduced pressure to obtain 450 mg (yield: 80%) of the title compound as an oil. The resulting compound was used in the next reaction without further purification.

WORKUP

后处理

  1. filtrationwas then filtered
  2. washwashed several times with ethyl acetate
  3. concentrationconcentrated under reduced pressure
  4. customto remove the organic solvent
  5. additionTo the residue were added methanol (60 ml) and 10% Pd/C (300 mg)
  6. stirringthe reaction mixture was stirred for 8 hours at 5 atomsphere under hydrogen gas
  7. additionEthyl acetate was added again to the reaction solution which
  8. filtrationwas then filtered
  9. concentrationconcentrated under reduced pressure