تفاعل #705105

ord-ebc31b839eaf403e99e56f2daef18775

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwere heated in a bomb on a steam bath for 4 hours
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    غسيلthe suspension was washed out of the bomb with 50 mL of methanol/water (50:50)
  4. 4
    أخرىthe solvents were evaporated in vacuo
  5. 5
    ترشيحfiltered
  6. 6
    أخرىcrystallized from ethanol

الإجراء التجريبي

A mixture of 3.4 g of 2-amino-7-chloro-6-(4-methoxyphenyl)-pyrido[2,3-d]pyrimidine from Example 12, 40 mL of anhydrous methylamine, and 10 mL of methanol were heated in a bomb on a steam bath for 4 hours. After cooling, the suspension was washed out of the bomb with 50 mL of methanol/water (50:50) and the solvents were evaporated in vacuo. The solid residue was slurried with 50 mL of water, filtered, and crystallized from ethanol to afford 2.2 g of the title compound 6-(4-methoxyphenyl)-N7 -methyl-pyrido[2,3-d]-pyrimidine-2,7-diamine, mp 270-275° C. dec.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05952342uspto-grants-1999_09