HRID1953774

反应详情

EQUATION

反应方程式

HRID 1953774 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

160 mg (0.37 mmol) of dimethyl N-(7-nitro-2,3-dimethoxyquinoxalin-5-ylmethyl)-α-(ethylamino)ethylphosphonate are dissolved in 8 ml of dichloromethane and stirred at room temperature for one hour with 0.19 ml (4 eq.) of triethylbromosilane. The solvent and excess reagent are evaporated and the residue is briefly dried in a high vacuum, dissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid, and stirred at room temperature for 18 hours. The reaction mixture is diluted with diethyl ether, and the solid is filtered off, washed with diethyl ether and dried. The title compound is obtained as a beige solid; m.p.=191° (dec.).

WORKUP

后处理

  1. customThe solvent and excess reagent are evaporated
  2. customthe residue is briefly dried in a high vacuum
  3. dissolutiondissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid
  4. additionThe reaction mixture is diluted with diethyl ether
  5. filtrationthe solid is filtered off
  6. washwashed with diethyl ether
  7. customdried