HRID429392

反应详情

EQUATION

反应方程式

HRID 429392 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Using the above procedure, 3,4-dihydroxybenzoic acid (0.0649 mole) and sodium hydroxide (0.0649 mole) were dissolved in 50% isopropyl alcohol (200 ml). Propargyl bromide (0.0649 mole) was added and the solution was heated to reflux for 6 hours. The solution was then cooled and the isopropyl alcohol was removed under vacuum. The residue was taken up in methylene chloride (200 ml), washed with water (200 ml), saturated sodium bicarbonate, saline and dried over magnesium sulfate. Removal of the solvent yielded crude product, which was recrystallized, from CCI4 to give the pure product. (68.0% yield) m.p. 127-129° C.

WORKUP

后处理

  1. temperaturethe solution was heated
  2. temperatureto reflux for 6 hours
  3. temperatureThe solution was then cooled
  4. customthe isopropyl alcohol was removed under vacuum
  5. washwashed with water (200 ml), saturated sodium bicarbonate, saline
  6. dry with materialdried over magnesium sulfate
  7. customRemoval of the solvent
  8. customyielded crude product, which
  9. customwas recrystallized, from CCI4
  10. customto give the pure product