HRID1590954

反应详情

EQUATION

反应方程式

HRID 1590954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureis heated
  2. temperatureat reflux for four hours
  3. customWater is collected in a Dean-Stark trap
  4. customThe liquid phase is decanted
  5. washresidual solids are washed with toluene
  6. dry with materialThe combined organic solutions are dried over magnesium sulfate
  7. concentrationconcentrated
  8. customto give a viscous oil
  9. customPurification by HPLC (Waters Prep. 500 A, 29:1 heptane:ethyl acetate)