HRID1033070

反应详情

EQUATION

反应方程式

HRID 1033070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-(5-aminomethylfuran-2-yl)-2-(diaminomethyleneamino)thiazole (1.6 g), imino(methylthio)methylcarbamic acid methylester (1.2 g) and triethylamine (1.5 g) was stirred at room temperature for 26 hours and then refluxed for 2.5 hours. Imino(methylthio)methylcarbamic acid methylester (1.0 g) was added to the reaction mixture and the mixture was refluxed for 10 hours. The solvent was removed under reduced pressure. The residue was chromatographed on a silica gel column eluting with a mixture of chloroform and methanol (10:1, V/V). Recrystallization from a mixture of methanol and diisopropyl ether afforded 2-(diaminomethyleneamino)-4-[5-(2-methoxycarbonylguanidino)methylfuran-2-yl]thiazole (530 mg).

WORKUP

后处理

  1. temperaturerefluxed for 2.5 hours
  2. temperaturethe mixture was refluxed for 10 hours
  3. customThe solvent was removed under reduced pressure
  4. customThe residue was chromatographed on a silica gel column
  5. washeluting with a mixture of chloroform and methanol (10:1, V/V)
  6. customRecrystallization
  7. additionfrom a mixture of methanol and diisopropyl ether