HRID2100352

反应详情

EQUATION

反应方程式

HRID 2100352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Bromo-3-chloro-5-methoxybenzene (Preparation 16, 6.0 g, 27 mmol) and trichloroisocyanuric acid (2.3 g, 9.9 mmol) were stirred in dimethylformamide (100 ml) at 50° C. for 3 hours. n-Heptane was added and the mixture filtered to remove insoluble impurities. The mixture was then concentrated in vacuo and the residue purified by silica gel column chromatography, eluting with n-heptane:ethyl acetate 9:1, to afford the title product as a white solid (5.0 g).

WORKUP

后处理

  1. filtrationthe mixture filtered
  2. customto remove insoluble impurities
  3. concentrationThe mixture was then concentrated in vacuo
  4. customthe residue purified by silica gel column chromatography
  5. washeluting with n-heptane:ethyl acetate 9:1