HRID1968518
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 solution of 2-(4-nitro-1H-pyrazol-1-yl)ethanol (1.08 g, 6.87 mmol) in methanol (34 ml) was evacuated and purged with nitrogen and treated with palladium on carbon (0.1 g, 0.094 mmol). The resulting black suspension was evacuated and purged with a hydrogen balloon and stirred under hydrogen overnight. The mixture was filtered through celite with methanol washes, and concentrated. The residue was flash chromatographed (50 mm; 9% methanol/methylene chloride w/0.1% NH4OH then 10% methanol/methylene chloride w/0.1% NH4OH) to afford the title compound.
WORKUP
后处理
- custompurged with nitrogen
- customThe resulting black suspension was evacuated
- custompurged with a hydrogen balloon
- filtrationThe mixture was filtered through celite with methanol washes
- concentrationconcentrated
- customchromatographed (50 mm