反应 #332463

ord-c337896fbc5a4a7cb17b2440f419168e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度at reflux for 12 h
  3. 3
    其他The cooled reaction mixture
  4. 4
    浓缩was concentrated
  5. 5
    其他the product was purified by flash chromatography on silica gel

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08658791B2uspto-grants-2014_02