HRID27313

反应详情

EQUATION

反应方程式

HRID 27313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 24.4 g of Cyclobutane carbinol (prepared in Example 42A) in 570 ml of dry pyridine was stirred under argon at -10° C. and 81.0 g of tosyl chloride added in small portions. The reaction mixture was stirred at -10° C. to -0° C. for 4.5 hr, then poured into 1 liter of chilled 6 N HCl. The layers were separated and the aqueous layer extracted with ether-ethyl acetate. The combined extracts were washed with 10% aqueous sodium bicarbonate (NaHCO3), dried (MgSO4), filtered and evaporated in vacuo to yield 72.0 g of the title compound having the following physical characteristics:

WORKUP

后处理

  1. customThe layers were separated
  2. extractionthe aqueous layer extracted with ether-ethyl acetate
  3. washThe combined extracts were washed with 10% aqueous sodium bicarbonate (NaHCO3)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo