HRID66969

反应详情

EQUATION

反应方程式

HRID 66969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.57 g. (0.0162 mole) of ethyl 3,3-dimethyl-7-chloroheptanoate in 100 ml. of methyl ethyl ketone is added 4 g. of sodium iodide and the mixture heated at reflux for 18 hours. The reaction mixture is cooled, filtered and concentrated. The residue is partitioned between ether and water. The aqueous phase is extracted several times with ether. The extract is washed with sodium bisulfite solution, water and saline. The organic solution is dried over magnesium sulfate and concentrated to give 4.182 g. of a yellow oil. The material is purified by distillation, b.p. 86°-87° C. (0.18 Torr).

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. temperatureThe reaction mixture is cooled
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue is partitioned between ether and water
  6. extractionThe aqueous phase is extracted several times with ether
  7. washThe extract is washed with sodium bisulfite solution, water and saline
  8. dry with materialThe organic solution is dried over magnesium sulfate
  9. concentrationconcentrated
  10. customto give 4.182 g
  11. distillationThe material is purified by distillation, b.p. 86°-87° C. (0.18 Torr)