HRID917470
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
To a stirred solution of 550 g (26.7 mmol) 2-(3,6-dihydro-2H-pyran-4-yl)-4-nitro-pyridine in 230 ml tetrahydrofuran and 5 ml glacial acetic acid was added 2.84 g of 10% palladium on charcoal and the mixture was then stirred for 16 h under an atmosphere of hydrogen at room temperature and 1.7 bar pressure. The mixture was then filtered, washing with methanol, and the filtrate concentrated in vacuo. Flash chromatography (methanol/dichloromethane/triethylamine 100/5/1) afforded 4.75 g (100%) 2-(tetrahydro-pyran-4-yl)-pyridin-4-ylamine as a light yellow oil. ES-MS m/e (%): 179 (M+H+, 100).
WORKUP
后处理
- filtrationThe mixture was then filtered
- washwashing with methanol
- concentrationthe filtrate concentrated in vacuo