HRID1413851

反应详情

EQUATION

反应方程式

HRID 1413851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.4 g of 3-methyl-5-[2-(2-hydroxy-3-chloropropoxy)-styryl]-isoxazole, 10 ml of tert.-butylamine and 50 ml of dioxane are heated for 10 hours at 100° C. in an autoclave. After distilling off the volatile constituents under reduced pressure, the very viscous crude product is partitioned between ether and 2 N sulfuric acid and the aqueous phase is cautiously rendered alkaline with 4 N sodium hydroxide solution and is finally extracted with ether. After drying the organic phase over sodium sulfate, the solvent is removed and the residue left is converted to 3-methyl-5-[2-(2-hydroxy-3-tert.-butylaminopropoxy)-styryl]-isoxazole hydrochloride, of melting point 216°-218° C., by the method described in Example 3.

WORKUP

后处理

  1. distillationAfter distilling off the volatile constituents under reduced pressure
  2. customthe very viscous crude product is partitioned between ether and 2 N sulfuric acid
  3. extractionis finally extracted with ether
  4. dry with materialAfter drying the organic phase over sodium sulfate
  5. customthe solvent is removed
  6. waitthe residue left