HRID1089216

反应详情

EQUATION

反应方程式

HRID 1089216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a dry flask were mixed 15 g of dry pyridine hydrochloride and 3.15 g (130 mmol) of 3-benzyl-2,4-dioxo-8-methyl-3,8-diazabicyclo [3.2.1] octane prepared according to U.S. Pat. No 3,328,398 in June 27, 1967. The mixture was heated in an oil bath preheated at 220° C. for 20 mn, cooled in an ice-bath, dissolved in 90 ml water, extracted four times with 100 ml ethyl ether. The organic layers were collected and dried over magnesium sulfate. After removing the solvent, the residue was chromatographed over silica-gel using dichloromethane/ethylacetate (80:20) to afford 1.5 g of the title compound (50%). M.P. 72° C.

WORKUP

后处理

  1. customprepared
  2. temperatureThe mixture was heated in an oil bath
  3. custompreheated at 220° C. for 20 mn
  4. temperaturecooled in an ice-bath
  5. extractionextracted four times with 100 ml ethyl ether
  6. customThe organic layers were collected
  7. dry with materialdried over magnesium sulfate
  8. customAfter removing the solvent
  9. customthe residue was chromatographed over silica-gel