반응 #3510

ord-2f0d5340aaf840a58a389a03ef389f8c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도were heated in a bomb on a steam bath for 4 hours
  2. 2
    온도After cooling
  3. 3
    세척the suspension was washed out of the bomb with 50 mL of methanol/water (50:50)
  4. 4
    기타the solvents were evaporated in vacuo
  5. 5
    여과filtered
  6. 6
    기타crystallized from ethanol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733913uspto-grants-1998_03