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
L-phenylalanine ethyl ester hydrochloride (1.0 g, 4.4 mmol) was added to a mixture of 2,4-dichloro-6-dihexylamino-1,3,5-triazine (1.5 g, 4.5 mmol) and sodium carbonate (0.92 g, 8.7 mmol) in acetonitrile (40 mL). The reaction mixture was heated to reflux for 16 h and then allowed to col to ambient temperature. The mixture was diluted with ethyl acetate and water. The phases were separated and the organic phase was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The crude material was purified by flash column chromatography through silica gel (elution with chloroform) to afford N-{4-chloro-6-(N,N-dihexylamino)-1,3,5-triazin-2-yl}phenylalanine ethyl ester. Anal. Calcd. for C26H40ClN5O2: C, 63.72; H, 8.23; N 14.29. Found: C, 63.67; H, 8.06; N, 14.24.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 16 h
- customto col to ambient temperature
- customThe phases were separated
- washthe organic phase was washed with brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe crude material was purified by flash column chromatography through silica gel (elution with chloroform)