HRID1389760

反应详情

EQUATION

反应方程式

HRID 1389760 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-benzyl-4-hydroxy-piperidine (19.2 g) in dry tetrahydrofuran (100 ml), sodium hydride (2.4 g, 0.1 mole) was added and the mixture was refluxed until evolution of hydrogen ceased (1 hour). A solution of ethyl bromoacetate (18.4 g) in dry tetrahydrofuran (20 ml) was added and the mixture was refluxed for 3 hours. After standing over night, the solvent was removed in vacuo and the residue was extracted with light petroleum. The extract was concentrated to a sirup which was distilled at 0.1 mm Hg to give (A) as a colourless oil with b.p. 140°-145° C.

WORKUP

后处理

  1. custom(1 hour)
  2. temperaturethe mixture was refluxed for 3 hours
  3. waitAfter standing over night
  4. customthe solvent was removed in vacuo
  5. extractionthe residue was extracted with light petroleum
  6. concentrationThe extract was concentrated to a sirup which
  7. distillationwas distilled at 0.1 mm Hg