HRID2352575

反应详情

EQUATION

反应方程式

HRID 2352575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 422 mg of 2-pyridylacetic acid hydrochloride and 596 μl of cyclohexylmethanol in 5 ml of dry pyridine was added 651 mg of 1,3-dicyclohexylcarbodiimide, and the mixture was stirred for 10 hours at room temperature. The precipitates were filtered off and the filtrate was evaporated under reduced pressure. The residue was dissolved in 20 ml of a 1N-hydrochloric acid, acidic solution was washed twice with 25 ml of diethyl ether. A 2N-aqueous sodium hydroxide was added to the solution to a pH of 11. A separated oil was extracted with 50 ml of dichloromethane, and the organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure to obtain 525 mg of cyclohexylmethyl 2-pyridylacetate as an oil.

WORKUP

后处理

  1. filtrationThe precipitates were filtered off
  2. customthe filtrate was evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in 20 ml of a 1N-hydrochloric acid, acidic solution
  4. washwas washed twice with 25 ml of diethyl ether
  5. additionA 2N-aqueous sodium hydroxide was added to the solution to a pH of 11
  6. extractionA separated oil was extracted with 50 ml of dichloromethane
  7. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  8. customthe solvent was evaporated under reduced pressure