تفاعل #1451126

ord-9454ac5f5e9746f7b27e85b965832301

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةat reflux for 12 hours
  3. 3
    أخرىThe cooled reaction mixture
  4. 4
    تركيزwas concentrated
  5. 5
    أخرىthe product was isolated by column chromatography

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07888287B2uspto-grants-2011_02