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With sodium ethanolate In ethanol at 20℃; for 0.5 h; Inert atmosphere
Methyl hydrazine acetate (403 mg, 3.87 mmol) was suspended in 15 mL of absolute ethanol solution and sodium ethoxide (395 mg, 5.81 mmol) was added. The reaction solution was stirred under nitrogen for 30 minutes at room temperature.Compound 37B (984 mg, 3.87 mmol) was dissolved in 10 mLIn the absolute ethanol, the solution was added dropwise to the stirred reaction system. After the addition is completed, the temperature is raised to the reflux temperature, under nitrogen protection.The reaction was stirred overnight. The reaction solution was quenched with water and the ethanol was spun off.The aqueous phase was extracted three times with ethyl acetate and dried.Purification with petroleum ether / ethyl acetate = 2:1 to give compound 37B as a yellow oil.(715 mg, 78percent yield).
Reference：
[1] Patent: CN108250128, 2018, A, . Location in patent: Paragraph 0648; 0650; 0653; 0654
Stage #1: tert-butyl-7,8-dihydropyrido[4,3-d]pyrimidin-6(5H)-carboxylate With trifluoroacetic acid In dichloromethane at 0 - 20℃; for 1h;
Stage #2: With ammonia In methanol
3
A solution of the product from Step B above (730 mg) in 10 mL of dichloromethane was cooled to 0 0C and treated dropwise with 5 mL of trifluoroacetic acid. The solution was warmed to room temperature and, after 1 h, concentrated under reduced pressure. The residue was dissolved in methanol and applied to an ion-exchange column (Varian Bond-Elut SCX, 5 g; preconditioned with methanol).The column was washed several times with methanol, and the amine product was eluted with 1.0M ammonia-methanol. The fractions containing product were concentrated under reduced pressure to afford the title compound as an orange oil. LC/MS 136.1 (M+l).
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