HRID2427470

反应详情

EQUATION

反应方程式

HRID 2427470 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Purge with N2 and H2 a mixture of 2-(4-benzyloxy-2,6-dichloro-benzyl)-2-aza-spiro[4.5]decan-1-one (1.18 g, 2.82 mmol) and 20% palladium (II) hydroxide on carbon (0.50 g) in ethyl acetate (100 mL) and stir under a balloon of H2 for 4 hours at room temperature. Add sodium sulfate to the mixture and filter through hyflo. Remove the solvent in vacuo and purify the crude product on silica isocratically with 9:1 chloroform:methyl t-butyl ether on silica gel to affort 0.72 g (78%) of the titled product. Rf=0.18 (9:1 chloroform:methyl t-butyl ether).

WORKUP

后处理

  1. customPurge with N2 and H2
  2. filtrationAdd sodium sulfate to the mixture and filter through hyflo
  3. customRemove the solvent in vacuo
  4. custompurify the crude product on silica isocratically with 9:1 chloroform