HRID1669571

反应详情

EQUATION

反应方程式

HRID 1669571 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2-dimethylnon-8-enoic acid ethyl ester (51, 800 mg, 3.77 mmol) and LiOH (806 mg, 18.9 mmol) in THF/MeOH/water, 1:1:0.5, was heated at 50° C. for 2.5 h. Then, additional LiOH (1.60 g, 10 eq) was added. After 15 h, the reaction mixture was concentrated under reduced pressure. The pH of the residue was adjusted to 3 with HCl 1N, extracted with CH2Cl2, washed with brine, dried (MgSO4), filtered and concentrated to give 650 mg (94%) of the title product (52) as a colorless oil.

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. extractionextracted with CH2Cl2
  3. washwashed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated