HRID2072475

反应详情

EQUATION

反应方程式

HRID 2072475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8-[(3,4-dihydro-2-naphthalenyl)methyl]-1,3,8-triazaspiro[4.5]dec-2-en-4-one (5.0 g) in dry tetrahydrofuran (30 ml) is added dropwise to a slurry of lithium aluminum hydride (0.5 g) in tetrahydrofuran (60 ml). The resulting mixture is refluxed under nitrogen for 16 hours. The reaction mixture is cooled and treated, in order, with water (0.6 ml), 15% sodium hydroxide solution (0.6 ml), and water (1.8 ml). The resulting mixture is stirred for 30 minutes. The mixture is filtered and the solids washed with chloroform. The filtrate is washed with brine, dried over sodium sulfate, and concentrated to give the title compound.

WORKUP

后处理

  1. temperatureThe resulting mixture is refluxed under nitrogen for 16 hours
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe mixture is filtered
  4. washthe solids washed with chloroform
  5. washThe filtrate is washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated