HRID40544

反应详情

EQUATION

反应方程式

HRID 40544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 34 ml of dichloromethane containing 0.9 g of tert-butyl ester of 4-tert-butoxyimino-piperidine-1-carboxylic acid is cooled to 0° C. 25 ml of a 4M solution of hydrochloric acid in dioxane (30 eq) is added. The reaction mixture is stirred at room temperature for 3 hours and then diluted by adding dichloromethane. A saturated solution of sodium hydrogen carbonate is then added until pH=8 is obtained. The aqueous phase is extracted three times with dichloromethane. The organic phases are then combined, dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. 0.49 g of piperidin-4-one O-tert-butyl-oxime is obtained.

WORKUP

后处理

  1. additiondiluted
  2. customis obtained
  3. extractionThe aqueous phase is extracted three times with dichloromethane
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure