تفاعل #3269

ord-9cc63b0f6a514bce8d35b9f03404b410

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux
  3. 3
    أخرىThe solvent was evaporated under reduced pressure
  4. 4
    أخرىthe residue was triturated with 20 mL of water
  5. 5
    ترشيحfiltered
  6. 6
    غسيلthe cake washed well with water
  7. 7
    أخرىPurification

الإجراء التجريبي

A mixture of 0.321 g (1.0 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7-(8H)-one from Example 12 and 0.404 g (1.0 mmol) of Lawesson's Reagent in 10 mL of pyridine was heated at reflux with stirring for 24 hours. The solvent was evaporated under reduced pressure, and the residue was triturated with 20 mL of water, filtered, and the cake washed well with water. Purification was by silica gel chromatography to afford the desired compound identified as 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]-pyrimidin-7(8H)-thione.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733914uspto-grants-1998_03