HRID1872073

反应详情

EQUATION

反应方程式

HRID 1872073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,3-Dihydro-1-methyl-5-nitrospiro[benzofuran-3,4'-piperidine](D4, 0.70 g, 2.8 mmol) and 4-chlorophenoxyacetonitrile (0.90 g, 5.4 mmol) were dissolved in dry DMF (15 ml) and added to potassium t-butoxide (1.60 g, 14.3 mmol). The mixture was stirred under Ar for 6h, diluted with water (150 ml), acidified (5M HCl) and washed with ethyl acetate. It was then basified (saturated K2CO3 solution) and extracted with ethyl acetate. This extract was dried (Na2SO4) and evaporated to give the title compound (0.35 g, 43%) still containing some spirocyclic starting material (ca 30%, NMR).

WORKUP

后处理

  1. washwashed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. dry with materialThis extract was dried (Na2SO4)
  4. customevaporated