HRID621387

反应详情

EQUATION

反应方程式

HRID 621387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionUpon complete addition
  2. stirringstirring
  3. filtrationThe precipitated product was filtered off (and
  4. customwas evaporated
  5. additionThe residue was treated with 2,2'-oxybispropane
  6. filtrationThe precipitated product was filtered off
  7. customBoth were crystallized from acetonitrile
  8. filtrationThe product was filtered off
  9. customdried