تفاعل #332463

ord-c337896fbc5a4a7cb17b2440f419168e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةat reflux for 12 h
  3. 3
    أخرىThe cooled reaction mixture
  4. 4
    تركيزwas concentrated
  5. 5
    أخرىthe product was purified by flash chromatography on silica gel

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08658791B2uspto-grants-2014_02