HRID1704734

反应详情

EQUATION

反应方程式

HRID 1704734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Phenoxy-2-propyl methane sulfonate (1 mole), anhydrous piperazine (4 moles) and potassium carbonate (2 moles) are added to 1000 ml methyl ethyl ketone. The mixture is refluxed during 45 hours, with stirring. The solvent is removed in vacuo and the residue is taken up into water and ether. The ethereal phase is again treated with a dilute aqueous hydrochloric acid solution and the aqueous phase is evaporated off. The resulting oil is taken up into a minimum amount of water. Sodium hydroxide (30 g) is added thereto, after which the material is extracted twice with ether. The ether is removed and the residual oil is distilled. B.p. = 104°-105° C./0.1 mm Hg. N.M.R.: consistent.

WORKUP

后处理

  1. temperatureThe mixture is refluxed during 45 hours
  2. customThe solvent is removed in vacuo
  3. additionThe ethereal phase is again treated with a dilute aqueous hydrochloric acid solution
  4. customthe aqueous phase is evaporated off
  5. additionSodium hydroxide (30 g) is added
  6. extractionafter which the material is extracted twice with ether
  7. customThe ether is removed
  8. distillationthe residual oil is distilled