HRID1943779
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 solution of (1S)-1-pyridin-3-ylbutan-1-amine (600 mg, 4.0 mmol) in ethanol (20 mL) was added 2,4-dichloro-5-methylpyrimidine (717 mg, 4.4 mmol) and diisopropylethylamine (1.4 mL, 8 mmol). The solution was heated at reflux for 24 h after which time the solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate (30 mL) and washed with H2O (2×15 mL), brine (15 mL) and dried (Na2SO4). The residue remaining after concentration in vacuo was chromatographed using ethyl acetate-hexanes (9:1) as eluant to separate the desired product (370 mg).
WORKUP
后处理
- temperatureThe solution was heated
- temperatureat reflux for 24 h after which time the solvent
- customwas removed under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate (30 mL)
- washwashed with H2O (2×15 mL), brine (15 mL)
- dry with materialdried (Na2SO4)
- concentrationafter concentration in vacuo
- customwas chromatographed
- customto separate the desired product (370 mg)