HRID26073

反应详情

EQUATION

反应方程式

HRID 26073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 600 mg. (1.98 mmoles) of 3-[4-(1,1-dimethylheptyl)-2-hydroxyphenyl]-piperidine, 0.78 ml. of 37% formaldehyde, 1.98 ml. of 1N hydrochloric acid and 150 mg. of 5% palladium-on-carbon is hydrogenated under 55 p.s.i. of hydrogen for 1.5 hours. The reaction mixture is filtered through diatomaceous earth and concentrated under reduced pressure. The residue is diluted with 75 ml. of saturated sodium bicarbonate and extracted with two 75 ml. portions of dichloromethane. The combined extract is washed with 75 ml. of saturated sodium chloride, dried over magnesium sulfate and evaporated to yield 567 mg. (90%) of the title compound as an oil.

WORKUP

后处理

  1. additionA mixture of 600 mg
  2. filtrationThe reaction mixture is filtered through diatomaceous earth
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue is diluted with 75 ml
  5. extractionof saturated sodium bicarbonate and extracted with two 75 ml
  6. extractionThe combined extract
  7. washis washed with 75 ml
  8. dry with materialof saturated sodium chloride, dried over magnesium sulfate
  9. customevaporated
  10. customto yield 567 mg