HRID846258

反应详情

EQUATION

反应方程式

HRID 846258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4-(4-hydroxyphenyl)-2-butanone (100 g) in 500 ml of ethanol with anhydrous dimethylamine (300 ml) and 5% palladium on sulfide carbon (100 g) was placed in a high pressure reaction vessel and kept under 1000 psi of H2 at 175° C. for 8 hours. The resultant solution was then filtered and the solvent removed in vacuo to give an oil which was dissolved in 1N hydrochloric acid (100 ml) and extracted with two 100 ml portions of ether. The aqueous layer was adjusted to pH7 with 2N sodium hydroxide and extracted with an additional two 100 ml volumes of ether. The organic extract was retained and dried and reduced in volume to give 55 g (47% yield) of the desired subtitled intermediate.

WORKUP

后处理

  1. filtrationThe resultant solution was then filtered
  2. customthe solvent removed in vacuo
  3. customto give an oil which
  4. extractionextracted with two 100 ml portions of ether
  5. extractionextracted with an additional two 100 ml volumes of ether
  6. extractionThe organic extract
  7. customdried