HRID434574

反应详情

EQUATION

反应方程式

HRID 434574 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Water (500 ml) and potassium dihydrogenphosphate (2.0 g) were placed in an autoclave, and the mixture was adjusted to pH 5.1 with an aqueous 1N NaOH solution at 30° C. α-Methylallyl-2-furylcarbinol (15 g) was then added, and the mixture was heated at 150° C. for 5.5 hours while stirring. After cooling, the reaction mixture was adjusted to pH 7.1 with an aqueous 1N NaOH solution at 30° C. and re-heated at 150° C. for 5 hours while stirring. After completion of the reaction, the mixture was admixed with sodium chloride (10 g) and extracted with methyl isobutyl ketone. The solvent was removed from the reaction mixture, and distillation of the resulting residue gave 2-(α-methylallyl)-4-hydroxy-2-cyclopentenone with the yield of 12 g (80%). B.P., 88°-90° C./0.12 mmHg.

WORKUP

后处理

  1. additionwas then added
  2. temperatureAfter cooling
  3. temperaturere-heated at 150° C. for 5 hours
  4. stirringwhile stirring
  5. customAfter completion of the reaction
  6. extractionextracted with methyl isobutyl ketone
  7. customThe solvent was removed from the reaction mixture, and distillation of the resulting residue