HRID1651335

反应详情

EQUATION

反应方程式

HRID 1651335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 200 ml portion of the above 4N hydrogen chloride solution in 1,4-dioxane was added to 35.0 g of tert-butyl 2-methoxyimino-3-oxobutyrate and the thus-obtained solution was stirred at 23° to 25° C. for 13 hours. The supernatant was concentrated, 200 ml of methylene chloride was added to the residue for dissolution of the latter, 30 ml of 20% aqueous sodium chloride was added to the thus-obtained supernatant, the mixture was shaken, and the organic layer was separated, dried over 12 g of anhydrous magnesium sulfate and concentrated to dryness under reduced pressure to give 21.8 g of 2-methoxyimino-3-oxobutyric acid.

WORKUP

后处理

  1. concentrationThe supernatant was concentrated
  2. addition200 ml of methylene chloride was added to the residue for dissolution of the latter, 30 ml of 20% aqueous sodium chloride
  3. additionwas added to the thus-obtained supernatant
  4. stirringthe mixture was shaken
  5. customthe organic layer was separated
  6. dry with materialdried over 12 g of anhydrous magnesium sulfate
  7. concentrationconcentrated to dryness under reduced pressure