HRID1869620

反应详情

EQUATION

反应方程式

HRID 1869620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1,1-Dimethylethyl 4-(4-pyridinylmethyl)-1-piperidinecarboxylate (may be prepared as described in Description 1) (11.4 g) was dissolved in ethanol (200 ml) and acetic acid (2.36 ml). Platinum oxide (2 g) was added under a blanket of argon, and the reaction shaken under hydrogen at 50 psi for 18 h. After carefully filtering off the platinum catalyst, the solvent was evaporated and the residue redissolved in ethyl acetate (50 ml) and washed with saturated sodium hydrogen carbonate solution (50 ml). The aqueous phase was extracted into ethyl acetate (2×50 ml) and the combined organics dried (Na2SO4) and evaporated to give the title compound (D2) as white solid (9.4 g).

WORKUP

后处理

  1. filtrationAfter carefully filtering off the platinum catalyst
  2. customthe solvent was evaporated
  3. dissolutionthe residue redissolved in ethyl acetate (50 ml)
  4. washwashed with saturated sodium hydrogen carbonate solution (50 ml)
  5. extractionThe aqueous phase was extracted into ethyl acetate (2×50 ml)
  6. dry with materialthe combined organics dried (Na2SO4)
  7. customevaporated