反应详情

7 g of platinum dioxide and 7 g of active carbon are suspended in 500 ml of glacial acetic acid and pre-hydrogenated. Subsequently, a solution of 36.8 g of 1-[3-(p-tert.butyl-phenyl)-2-methyl-propyl]-piperidine in 1000 ml of glacial acetic acid and 67 ml of perchloric acid is added and the mixture is hydrogenated at 25° C. The catalyst is removed by filtration and the filtrate is treated with 110 g of potassium acetate dissolved in 100 ml of water. The precipitated potassium perchlorate is filtered, and the filtrate is evaporated on a rotary evaporator. The crystalline residue is made alkaline with 2-N sodium hydroxide, the free base is extracted with 500 ml of ether, washed neutral with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 1-[3-(4-tert.butyl-cyclohexyl)-2-methyl-propyl]-piperidine of boiling point 102° C./0.02 Torr.

1. customis hydrogenated at 25° C
2. customThe catalyst is removed by filtration
3. additionthe filtrate is treated with 110 g of potassium acetate
4. dissolutiondissolved in 100 ml of water
5. filtrationThe precipitated potassium perchlorate is filtered
6. customthe filtrate is evaporated on a rotary evaporator
7. extractionthe free base is extracted with 500 ml of ether
8. washwashed neutral with water
9. dry with materialdried over sodium sulphate
10. customevaporated
11. distillationBy distillation there