HRID626801

反应详情

EQUATION

反应方程式

HRID 626801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of [1-(4-azido-5-fluoropyridin-3-yl)meth-(E)-ylidene]-(4-bromo-2,6-dichlorophenyl)amine (˜60 mmol) in toluene (200 mL) was heated at 105° C. for 2 hours. The resultant mixture was cooled to room temperature and concentrated under reduced pressure. The residue was triturated with diethyl ether and the solid obtained was collected by filtration and dried to afford the title compound (14.5 g, 67% yield over two steps). 1H NMR (400 MHz, DMSO-d6): δ 9.25 (d, J=2.7 Hz, 1H), 9.20 (d, J=2.6 Hz, 1H), 8.28 (dd, J=3.8, 0.5 Hz, 1H), 8.19 (s, 2H).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was triturated with diethyl ether
  3. customthe solid obtained
  4. filtrationwas collected by filtration
  5. customdried