HRID1246802

反应详情

EQUATION

反应方程式

HRID 1246802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

6-Chloro-N4-(4-chlorophenyl)-pyrimidine-4,5-diamine I-(1A-1)a (114 mg, 0.45 mmol) and pyrrolidine (1 ml, excess) were combined and heated with stirring at 100° C. for 2 hours. The reaction mixture was diluted with saturated NaHCO3 solution and extracted with ethyl acetate. The organic layers were combined, dried (Na2SO4), filtered, and evaporated to dryness to yield the desired compound I-(17A-1)a (131 mg, quantitative) as an orange-brown solid: +ESI MS (M+1) 290.3; 1H NMR (500 MHz, CD3OD) δ 7.85 (s, 1H), 7.45 (d, J=8.8 Hz, 2H), 7.26 (d, J=8.8 Hz, 2H), 3.63 (m, 4H), 1.96 (m, 4H).

WORKUP

后处理

  1. temperatureheated
  2. extractionextracted with ethyl acetate
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated to dryness