HRID1036733

反应详情

EQUATION

反应方程式

HRID 1036733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution comprising tert-butyl 2-methyl-1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate (1.2 g, 3.63 mmol) and TFA (1.399 ml, 18.16 mmol) in DCM (20 ml) was stirred at RT for 4 days. The reaction mixture was concentrated in vacuo and the resulting crude product was dissolved with methanol (5 ml) and passed through a 10 g SCX-2 cartridge. The product was eluted with 2M NH3 in methanol (70 ml) and the relevant fractions were combined and concentrated in vacuo to afford the title compound as a yellow oil;

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionthe resulting crude product was dissolved with methanol (5 ml)
  3. washThe product was eluted with 2M NH3 in methanol (70 ml)
  4. concentrationconcentrated in vacuo