HRID2079833

反应详情

EQUATION

反应方程式

HRID 2079833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of carboxamide 1-E (0.64 g, 1.7 mmol) and cyanuric chloride (0.47 g, 2.53 mmol) in DMF (15 ml) was stirred at room temperature under a nitrogen atmosphere. After 2 h, DMF was removed in vacuo and the solid was redissolved in methylene chloride (100 ml). This solution was washed with saturated aqueous sodium bicarbonate and brine, dried (Na2SO4), and stripped to give 1-F as a pale yellow solid. MS (ESI+)=361.3 (M+1); 1H NMR (500 MHz, CDCl3): δ2.15 (6H, m), 2.22 (6H, m), 3.47 (3H, s), 7.51 (1H, m), 7.72 (2H, m), 7.87 (1H, m) ppm.

WORKUP

后处理

  1. customDMF was removed in vacuo
  2. dissolutionthe solid was redissolved in methylene chloride (100 ml)
  3. washThis solution was washed with saturated aqueous sodium bicarbonate and brine
  4. dry with materialdried (Na2SO4)