HRID1648516

反应详情

EQUATION

反应方程式

HRID 1648516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl Z-4-[[2-butyl-5-[(1-butyl-2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate (0.569 g, 1.2 mmol) in DMF (5 mL) is added K2CO3 (2.0 g, 15 mmol). After stirring for 5 minutes 2-amino-4-chloromethylthiazole hydrochloride (0.222 g, 1.2 mmol) is added. The mixture is stirred for 48 hours and then filtered. The filtrate is concentrated in vacuo and dissolved in methylene chloride (30 mL). This solution is washed with water and dried over K2CO3 and charcoal. A viscous oil is obtained by evaporation of the solvents in vacuo. This oil is dissolved in ether and treated with ethereal HCl to precipitate a gum which is collected by decantation. This gum is recrystallized from 2-propanol/ether.

WORKUP

后处理

  1. additionis added
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated in vacuo
  4. dissolutiondissolved in methylene chloride (30 mL)
  5. washThis solution is washed with water
  6. dry with materialdried over K2CO3 and charcoal
  7. customA viscous oil is obtained by evaporation of the solvents in vacuo
  8. customto precipitate a gum which
  9. customis collected by decantation
  10. customThis gum is recrystallized from 2-propanol/ether