HRID621387
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
To a stirred and heated (<40° C.) solution of 96 parts of decahydro-2,2-dimethyl-1-naphthalenamine in 400 parts of ethanol were added dropwise 48 parts of ethyl N-cyanomethanimidate. Upon complete addition, stirring was continued for 2 hours. The precipitated product was filtered off (and set aside) and the filtrate was evaporated. The residue was treated with 2,2'-oxybispropane. The precipitated product was filtered off and combined with the product, which was set aside (see above). Both were crystallized from acetonitrile. The product was filtered off and dried, yielding 67 parts (54.1%) of N'-cyano-N-(decahydro-2,2-dimethyl-1-naphthalenyl)methanimidamide; mp. 227.6° C. (intermediate 7).
WORKUP
后处理
- additionUpon complete addition
- stirringstirring
- filtrationThe precipitated product was filtered off (and
- customwas evaporated
- additionThe residue was treated with 2,2'-oxybispropane
- filtrationThe precipitated product was filtered off
- customBoth were crystallized from acetonitrile
- filtrationThe product was filtered off
- customdried