HRID1517578
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
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A mixture of 1-(3-fluoro-2-pyridyl)-3-methyl-pyrazole-4-carbaldehyde (230 mg, 1.12 mmol) and morpholine (2 mL, 22.93 mmol) is heated under microwave irradiation (temperature 160° C., ramp time: 2 min, hold time: 10 min, potency: 250 W). The excess of morpholine is eliminated in vacuo and the residue is diluted in dichloromethane and washed in saturated aqueous solution of sodium bicarbonate. The organic layer is separated, dried over magnesium sulfate and the solvent evaporated in vacuo. The residue is purified by normal phase Isco chromatography using hexane/ethyl acetate as eluent (from 50 to 100% in ethyl acetate) to yield 72% of the title compound. MS (m/z): 273 (M+1).
WORKUP
后处理
- washwashed in saturated aqueous solution of sodium bicarbonate
- customThe organic layer is separated
- dry with materialdried over magnesium sulfate
- customthe solvent evaporated in vacuo
- customThe residue is purified by normal phase Isco chromatography