HRID440719

反应详情

EQUATION

反应方程式

HRID 440719 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of E-5-(2-bromovinyl)-2,4-dimethoxypyrimidine (2.45 g; 10 mmol) in AcOH (10 ml) was added NaI (3.3 g; 2.2 eq.; 22 mmol) and the solution heated under reflux for 3 h. The hot mixture was filtered and diluted with water (15 ml). After cooling, the precipitated product was filtered off, washed with acetone (50 ml) and ether (20 ml) and dried to give a pale yellow powder (1.40 g, 65%). Mp>320° C.; 60 MHz 1H-NMR, DMSO-6d, δ: 7.60 (s, 1H, H-6); 7.30 (d, 1H, J=13 Hz, vinyl H); 6.80 (d, 1H, J=13 Hz, vinyl H).

WORKUP

后处理

  1. temperaturethe solution heated
  2. temperatureunder reflux for 3 h
  3. filtrationThe hot mixture was filtered
  4. additiondiluted with water (15 ml)
  5. temperatureAfter cooling
  6. filtrationthe precipitated product was filtered off
  7. washwashed with acetone (50 ml) and ether (20 ml)
  8. customdried