HRID1355546

反应详情

EQUATION

反应方程式

HRID 1355546 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-(2-Ethoxy-vinyl)-2-methylsulfanyl-pyrimidine (18-2, 0.236 g, 1.20 mmol) was dissolved in 5 mL EtOH and the resulting solution was cooled to 0° C. NBS (0.214 g, 1.20 mmol) was added in small portions. After 2 h the reaction was concentrated in vacuo. Purification by flash column chromatography (eluting with 98:2 DCM/MeOH) provided the titled compound. 1H NMR (CDCl3) δ 8.50 (d, 1H, J=5.0 Hz), 7.09 (d, 1H, J=5.1 Hz), 5.05 (d, 1H, J=6.8 Hz), 4.81 (d, 1H, J=6.9 Hz), 3.77 (m, 2H), 3.53 (m, 2H), 2.57 (s, 3H), 1.26 (t, 3H, J=7.0 Hz), 1.08 t, 3H, J=7.1 Hz).

WORKUP

后处理

  1. concentrationAfter 2 h the reaction was concentrated in vacuo
  2. customPurification
  3. washby flash column chromatography (eluting with 98:2 DCM/MeOH)