HRID1030005

反应详情

EQUATION

反应方程式

HRID 1030005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

7.1 g of β-methoxyethyl 6-fluoro-2-isocyanatosulfonylbenzoate in 20 ml of methylene chloride were added over 10 minutes at 25° C. to a stirred mixture of 4 g of 2-amino-4,6-dimethoxy-1,3,5-triazine in 40 ml of DMF under nitrogen; the temperature rose to 32° C. After the mixture had been stirred for 14 hours at 25° C., the solvent was removed under reduced pressure and the residue was stirred with ether and twice with 3N HCL. It was then taken up in acetone, insoluble mater was separated off and the filtrate was concentrated to dryness. 7 g of the compound shown in the title, of melting point 179° C.-182° C. were obtained.

WORKUP

后处理

  1. customrose to 32° C
  2. customthe solvent was removed under reduced pressure
  3. stirringthe residue was stirred with ether and twice with 3N HCL
  4. custominsoluble mater was separated off
  5. concentrationthe filtrate was concentrated to dryness
  6. customwere obtained