HRID846550

反应详情

EQUATION

反应方程式

HRID 846550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After 46.4 g of concentrated sulfuric acid and 21.2 g (147 mmol) of (-)-2-methyloctanol were added to 330 ml of water, 63.4 g (401 mmol) of potassium permanganate was added dropwise over 7.3 hours while the reaction temperature was held at 21°~28° C. The thus obtained reaction mixture was poured into 270 ml of ice water, added with 52 g of sodium hydrogen sulfite, adjusted to pH of not more than 1 with hydrochloric acid, extracted with ether and then extracted with a 10% aqueous solution of sodium hydroxide. This extract was added with hydrochloric acid to adjust pH to not more than 1 and again extracted with chloroform. The extract was washed with water, dried, concentrated and distilled under a reduced pressure (0.28 mmHg, 91°~94° C.) to obtain 15.3 g (yield 64%) of (+)-2-methyl octanoic acid.

WORKUP

后处理

  1. additionwas added dropwise over 7.3 hours while the reaction temperature
  2. customwas held at 21°~28° C
  3. customThe thus obtained reaction mixture
  4. extractionextracted with ether
  5. extractionextracted with a 10% aqueous solution of sodium hydroxide
  6. additionThis extract was added with hydrochloric acid
  7. extractionagain extracted with chloroform
  8. washThe extract was washed with water
  9. customdried
  10. concentrationconcentrated
  11. distillationdistilled under a reduced pressure (0.28 mmHg, 91°~94° C.)