反应 #1584076

ord-9247b934058e48959a71039e7caed1c4

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 hours
  3. 3
    其他The cooled reaction mixture
  4. 4
    浓缩was concentrated
  5. 5
    其他the product was isolated by column chromatography

实验过程

6-Amino-2-(4-chloro-2-fluoro-3-methoxy-phenyl)-pyrimidine-4-carboxylic acid methyl ester (778 mg, 2.5 mmol) and N-bromosuccinimide (489 mg, 2.75 mmol) were combined in chloroform and heated at reflux for 12 hours. The cooled reaction mixture was concentrated and the product was isolated by column chromatography to yield 6-amino-5-bromo-2-(4-chloro-2-fluoro-3-methoxyphenyl)pyrimidine-4-carboxylic acid methyl ester (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: US09199943B2uspto-grants-2015_12