HRID346294

反应详情

EQUATION

反应方程式

HRID 346294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into a reaction vessel equipped with a stirrer, condenser and thermometer was placed 0.2 mole of 5-hydroxyisophthalic acid. Thereto were added 0.6 mole of allyl alcohol, 300 ml of toluene, 1.3 g of sulfuric acid and 0.2 g of p-methoxyphenol and the mixture was refluxed with heating. A mixture of toluene and water was distilled off and cooled with a condenser, and toluene was separated from water and returned contineously to the reaction vessel. The mixture was heated for 8 hours and then allowed to cool. At this point, total of distilled water was 7 ml. After the reaction mixture was washed with a saturated aqueous solution of sodium chloride until the aqueous layer did not indicate acidic, toluene was distilled at a reduced pressure. The resulting concentrate was distilled at a reduced pressure to obtain 27 g (yield 52%) of diallyl 5-hydroxyisophthalate. b.p. 202°~205° C./5 mm Hg.

WORKUP

后处理

  1. customInto a reaction vessel equipped with a stirrer, condenser
  2. temperaturethe mixture was refluxed
  3. temperaturewith heating
  4. distillationwas distilled off
  5. temperaturecooled with a condenser
  6. customtoluene was separated from water
  7. temperatureThe mixture was heated for 8 hours
  8. temperatureto cool
  9. washAfter the reaction mixture was washed with a saturated aqueous solution of sodium chloride until the aqueous layer
  10. distillationtoluene was distilled at a reduced pressure
  11. concentrationThe resulting concentrate
  12. distillationwas distilled at a reduced pressure