반응 #3510
ord-2f0d5340aaf840a58a389a03ef389f8c
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도were heated in a bomb on a steam bath for 4 hours
- 2온도After cooling
- 3세척the suspension was washed out of the bomb with 50 mL of methanol/water (50:50)
- 4기타the solvents were evaporated in vacuo
- 5여과filtered
- 6기타crystallized 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.