HRID1590954
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 10.0 g (13.7 mmol) of 2-chloro-4,6-bis[N-(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl)-n-butylamino]-1,3,5-triazine (see Example 75), 1.43 g (16.4 mmol) of morpholine, 0.8 g of sodium hydroxide, and 30 g of toluene is heated at reflux for four hours. Water is collected in a Dean-Stark trap. The liquid phase is decanted and residual solids are washed with toluene. The combined organic solutions are dried over magnesium sulfate and concentrated to give a viscous oil. Purification by HPLC (Waters Prep. 500 A, 29:1 heptane:ethyl acetate) affords 5.9 g (55% yield) of the title compound, a white powder, m.p. 159°-63° C.
WORKUP
后处理
- temperatureis heated
- temperatureat reflux for four hours
- customWater is collected in a Dean-Stark trap
- customThe liquid phase is decanted
- washresidual solids are washed with toluene
- dry with materialThe combined organic solutions are dried over magnesium sulfate
- concentrationconcentrated
- customto give a viscous oil
- customPurification by HPLC (Waters Prep. 500 A, 29:1 heptane:ethyl acetate)