HRID245281

反应详情

EQUATION

反应方程式

HRID 245281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Amino-2-(4-chloro-2-fluoro-3-methoxyphenyl)pyrimidine-4-carboxylic acid methyl ester (778 mg, 2.5 mmol) and N-bromosuccinimide (489 mg, 2.75 mmol) were combined in chloroform (10 mL) and heated at reflux for 12 h. The cooled reaction mixture was concentrated and the product was purified by flash chromatography on silica gel to yield the title compound (752 mg, 77% yield): mp 173-175° C.: 1H NMR (CDCl3) δ 7.66 (dd, 1H), 7.24 (dd, 1H), 5.73 (br s, 2H), 4.03 (s, 3H), 4.01 (d, 3H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 12 h
  3. customThe cooled reaction mixture
  4. concentrationwas concentrated
  5. customthe product was purified by flash chromatography on silica gel