HRID1033050

反应详情

EQUATION

反应方程式

HRID 1033050 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(5-aminomethylfuran-2-yl)-2-(diaminomethyleneamino)thiazole (7.00 g) and dimethyl N-cyanodithioiminocarbonate (4.31 g) in N,N-dimethylformamide (70 ml) was stirred at 70° C. for two hours. 40% Aqueous methylamine by weight (14 ml) was added to the warmed solution and the mixture was stirred for an additional one hour at the same temperature. After the solvent was evaporated in vacuo, the residue was chromatographed on alumina, eluting with a mixture of chloroform and methanol (9:1, V/V), followed by recrystallization from a mixture of methanol, tetrahydrofuran and diisopropyl ether to afford 2-(diaminomethyleneamino)-4-[5-(2-cyano-3-methylguanidino)methylfuran-2-yl]thiazole (4.05 g).

WORKUP

后处理

  1. customAfter the solvent was evaporated in vacuo
  2. customthe residue was chromatographed on alumina
  3. washeluting with a mixture of chloroform and methanol (9:1, V/V)
  4. customfollowed by recrystallization from a mixture of methanol, tetrahydrofuran and diisopropyl ether