HRID478282

反应详情

EQUATION

反应方程式

HRID 478282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from Example 39A (3.1 g, 6.3 mmol) in chloroform (50 mL) was cooled to 0° C., treated with 90% pyridinium tribromide (2.45 g, 6.9 mmol), warmed to abmient temperature, stirred for 16 hours and washed with water. The chloroform layer was isolated, dried (MgSO4), filtered, refluxed for 16 hours and cooled in an ice bath. The resulting precipitate was collected by filtration and dried to provide the title compound (2.1 g) as tan crystals.

WORKUP

后处理

  1. temperaturewarmed
  2. washwashed with water
  3. customThe chloroform layer was isolated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. temperaturerefluxed for 16 hours
  7. temperaturecooled in an ice bath
  8. filtrationThe resulting precipitate was collected by filtration
  9. customdried