HRID1285123

反应详情

EQUATION

反应方程式

HRID 1285123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.3 g of the chlorine compound of Example 18 are dissolved in 60 ml of normal butanol, and 8 g of N-(2-aminoethyl)-morpholine are added. The mixture is heated under reflux for 3 hours and then poured into 1000 ml of water. The organic phase is extracted with ether and the ether solution is then extracted with a 1N solution of sulphuric acid. The aqueous phase is separated off, rendered alkaline with sodium hydroxide and extracted with ether. The ether phase is dried over magnesium sulphate and the solvent is then evaporated off to dryness in vacuo. This gives a yellow solid. Yield 81.3%; melting point 138° C.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. extractionThe organic phase is extracted with ether
  4. extractionthe ether solution is then extracted with a 1N solution of sulphuric acid
  5. customThe aqueous phase is separated off
  6. extractionextracted with ether
  7. dry with materialThe ether phase is dried over magnesium sulphate
  8. customthe solvent is then evaporated off to dryness in vacuo
  9. customThis gives a yellow solid