HRID971706

反应详情

EQUATION

反应方程式

HRID 971706 的结构方程式

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

Using the procedure of Example 17, 12 g of phosphorous oxychloride were slowly added to a mixture of 12 g of 3-methyl-1,2,4-oxadiazol-5-yl-acetic acid and 8.9 g of dry sec.-butanol and the rate of addition was adjusted to a reaction temperature of 65°±5° C. The resulting reaction mixture was stirred for 90 minutes at 65° C., and then treated as in Example 17. The product was distilled at 68° C. and 1.5 mm Hg to obtain 6.1 g (35% yield) of sec.-butyl 3-methyl-1,2,4-oxadiazol-5-yl-acetate. The purity of the final product was about 95% (according to TLC and PMR spectrum) and it had a refractive index nD25 =1.438.

WORKUP

后处理

  1. additionthe rate of addition
  2. customwas adjusted to a reaction temperature of 65°±5° C
  3. customThe resulting reaction mixture
  4. additiontreated as in Example 17
  5. distillationThe product was distilled at 68° C.