HRID577586
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of methyl 5-(2-aminoethoxy)-3-methyl-2-(propan-2-yloxy)pyridine-4-carboxylate (131e, 1.2 g, 2.2 mmol) and NaOEt (3.0 g, 45 mmol) in dry EtOH (60 mL) was refluxed for 14 hours. The reaction mixture was concentrated under vacuum. The residue was dissolved in H2O (30 mL) and extracted with EtOAc (2×20 mL). The combined organic layers were washed with brine (30 mL), dried over Na2SO4, and concentrated under vacuum to give 6-methyl-7-(propan-2-yloxy)-3,4-dihydropyrido[4,3-f][1,4]oxazepin-5(2H)-one (131f, 0.34 g) as a brown solid.
WORKUP
后处理
- temperaturewas refluxed for 14 hours
- concentrationThe reaction mixture was concentrated under vacuum
- dissolutionThe residue was dissolved in H2O (30 mL)
- extractionextracted with EtOAc (2×20 mL)
- washThe combined organic layers were washed with brine (30 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum