HRID745850

反应详情

EQUATION

反应方程式

HRID 745850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4.88 g of 2-[[(5-methyl-1H-imidazol-4-yl)methyl]thio]ethanamine (prepared according to British Pat. No. 1,338,169 which is hereby incorporated by reference,) in 75 ml of absolute ethanol, are added 5.55 ml of triethylamine. Then 1.96 g of ethyl N-cyano-formimidate in 15 ml of ethanol are added dropwise under stirring and at room temperature (prepared according to Huffman and Schaefer "J.Org.Chem.",28, 1816, 1963). Stirring is continued for 1 hour, after which are added 2.5 ml of 8N HCl/ethanol. A white solid is separated, which is subsequently crystallized in ethanol, filtered off and dried in a vacuum dessicator in the presence of phosphorus pentoxide and sodium hydroxide. 2.9 g of N-cyano-N'-[2-[[(5-methyl-1H-imidazol-4-yl)methyl]thio]ethyl]formamidine are obtained.

WORKUP

后处理

  1. custom(prepared according to Huffman and Schaefer "J.Org.Chem.",28, 1816, 1963)
  2. stirringStirring
  3. customA white solid is separated
  4. customwhich is subsequently crystallized in ethanol
  5. filtrationfiltered off
  6. dry with materialdried in a vacuum dessicator in the presence of phosphorus pentoxide and sodium hydroxide