反应详情

温度

80 °C

To a solution of cis-N-isopropyl-4-(5-nitro-2-(2-(piperidin-1-yl)ethoxy)pyridin-4-ylamino)cyclohexanecarboxamide (10.79 g, 24.89 mmol) in MeOH (124 mL) was added tin (II) chloride (18.88 g, 100 mmol), and the reaction was stirred at 80° C. for 2 hours. The reaction mixture was concentrated in vacuo, and the residue was dissolved in EtOAc, then diluted with 1N aqueous NaOH. The layers were separated, and the organic layer was washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo to yield cis-4-(5-amino-2-(2-(piperidin-1-yl)ethoxy)pyridin-4-ylamino)-N-isopropylcyclohexanecarboxamide (8.06 g, 80% yield). MS m/z=404.2 [M+H], calc 403.56 for C22H37N5O2.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionthe residue was dissolved in EtOAc
3. additiondiluted with 1N aqueous NaOH
4. customThe layers were separated
5. washthe organic layer was washed with brine
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo