Реакция #3510

ord-2f0d5340aaf840a58a389a03ef389f8c

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwere heated in a bomb on a steam bath for 4 hours
  2. 2
    ТемператураAfter cooling
  3. 3
    Промывкаthe suspension was washed out of the bomb with 50 mL of methanol/water (50:50)
  4. 4
    Другоеthe solvents were evaporated in vacuo
  5. 5
    Фильтрацияfiltered
  6. 6
    Другоеcrystallized from ethanol

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05733913uspto-grants-1998_03