HRID436683

反应详情

EQUATION

反应方程式

HRID 436683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 20.5 g. portion of the intermediate prepared in Example 1 and 10 g. of NaCN were added to 50 ml. of dimethylsulfoxide and heated at 110° C. for two hours. The reaction mixture was then cooled and poured into 300 ml. of water, which was then extracted with a total of 1 liter of ethyl ether. The combined ether extracts were dried over anhydrous Na2SO4, filtered, and evaporated to dryness yielding a dark oil. The oil was chromatographed on a silica gel column, eluting with ethyl acetate. The desired intermediate product, 5-(2-cyano-1,1-dimethylethyl)-2-methylamino-1,3,4-thiadiazole, m.p. 65°-67° C., was isolated in the amount of 750 mg.

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled
  2. additionpoured into 300 ml
  3. extractionof water, which was then extracted with a total of 1 liter of ethyl ether
  4. dry with materialThe combined ether extracts were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customyielding a dark oil
  8. customThe oil was chromatographed on a silica gel column
  9. washeluting with ethyl acetate