HRID1263169

反应详情

EQUATION

反应方程式

HRID 1263169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product from Example 1 (10.6 g), 2,3-dihydroxy butane (8.5 g) and p-toluene sulfonic acid (1.5 g) in 200 ml benzene were refluxed to 2 hours, removing water with a Dean Stark trap. The solution wash washed with 10% NaOH, dried (MgSO4) and stripped. The product was chromatographed on a silica gel column, eluting with 30% ethyl ether:hexane. Yield: 3.8 g of the title product, mp 55°-57° C.

WORKUP

后处理

  1. customremoving water with a Dean Stark trap
  2. washThe solution wash
  3. washwashed with 10% NaOH
  4. dry with materialdried (MgSO4)
  5. customThe product was chromatographed on a silica gel column
  6. washeluting with 30% ethyl ether