HRID478263

反应详情

EQUATION

反应方程式

HRID 478263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-benzylpiperidine-3,5-dione (Ziegler, J. Amer. Chem. Soc. (1973), 95, 7458-7464) (0.55 g, 2.5 mmol) in ethyl alcohol (5 mL) was treated with 2.0M ammonia in ethyl alcohol (1.25 mL, 2.5 mmol), stirred for 30 minutes in a sealed tube, treated with tetrahydrothiopyran-3-one-1,1-dioxide (0.36 g, 2.5 mmol), treated with 3-bromo-4-fluorobenzaldehyde (0.51 g, 2.5 mmol), stirred at 75° C. for 48 hours, cooled and concentrated. The residue was purified by flash chromatography over silica gel (5% ethanol/methylene chloride) to provide the title compound (0.50 g).

WORKUP

后处理

  1. stirringstirred at 75° C. for 48 hours
  2. temperaturecooled
  3. concentrationconcentrated
  4. customThe residue was purified by flash chromatography over silica gel (5% ethanol/methylene chloride)