HRID1033062

反应详情

EQUATION

反应方程式

HRID 1033062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

An ice-cooling mixture of 4-(5-aminomethylfuran-2-yl)-2-(diaminomethyleneamino)thiazole (0.8 g), 3-chlorobenzoisothiazol-1,1-dioxide (0.8 g) and triethylamine (0.5 ml) in N,N-dimethylformamide (15 ml) was stirred for 3 hours. To a reaction mixture was added a mixture of ethylacetate, tetrahydrofuran and water and the mixture was adjusted to pH 9.5 with 20% aqueous potassium carbonate. The separated organic layer was washed with brine and dried over magnesium sulfate. The solvent was removed by concentration and a residue was recrystallized from a mixture of methanol, dioxane and diisopropyl ether to give 2-(diaminomethyleneamino)-4-[5-(1,1-dioxobenzoisothiazol-3-yl)aminomethylfuran-2-yl]thiazole (0.49 g).

WORKUP

后处理

  1. additionTo a reaction mixture was added
  2. washThe separated organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed by concentration
  5. customa residue was recrystallized from a mixture of methanol, dioxane and diisopropyl ether