HRID2079833
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customDMF was removed in vacuo
- dissolutionthe solid was redissolved in methylene chloride (100 ml)
- washThis solution was washed with saturated aqueous sodium bicarbonate and brine
- dry with materialdried (Na2SO4)