HRID1501226

反应详情

EQUATION

反应方程式

HRID 1501226 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

To a solution of 1-(4-bromophenyl)ethanol (1 g, 5 mmol) in 20 mL of anhydrous N,N-dimethylformamide was added sodium hydride (0.36 g, 15 mmol) at room temperature and then stirred for 1 hour, 4-chloropyrimidine hydrochloride (1 g, 6 mmol) was added, and then heated at 100° C. for 12 hours. The reaction mixture was concentrated, the residue was purified by chromatography with petroleum/ethyl acetate=1:1 to afford 4-(1-(4-bromophenyl)ethoxy)pyrimidine (1.2 g, 86% yield). LRMS (M+H+) m/z: calcd for 278.01. found 278. 1H NMR (300 MHz, CD3OD) δ 8.65 (s, 1H), 8.42 (d, J=6.0 Hz, 1H), 7.48 (d, J=8.4 Hz, 2H), 7.35 (d, J=8.4 Hz, 2H), 6.92 (dd, J=6.0 and 1.2 Hz, 1H), 6.26 (q, J=6.6 Hz, 1H), 1.64 (d, J=6.6 Hz, 3H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue was purified by chromatography with petroleum/ethyl acetate=1:1