HRID436683
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was then cooled
- additionpoured into 300 ml
- extractionof water, which was then extracted with a total of 1 liter of ethyl ether
- dry with materialThe combined ether extracts were dried over anhydrous Na2SO4
- filtrationfiltered
- customevaporated to dryness
- customyielding a dark oil
- customThe oil was chromatographed on a silica gel column
- washeluting with ethyl acetate