HRID1948140

反应详情

EQUATION

反应方程式

HRID 1948140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Alternatively the compound could be obtained by heating 14.2 g of 8-methyl-1,4-dioxa-spiro[4.5]decane-8-carbonitrile in 190 mL of 80% acetic acid under reflux until conversion was complete. The mixture was cooled and poured onto 1.2 L of cold, saturated sodium bicarbonate solution. 600 mL of brine were added and the mixture was extracted several times with ethyl acetate. The combined ethyl acetate layers were washed with brine, dried over magnesium sulphate and evaporated. The residue was taken up in water and acetonitrile and lyophilized to give 6.75 g of the desired product, that could be directly used in further conversions.

WORKUP

后处理

  1. customAlternatively the compound could be obtained
  2. temperatureunder reflux until conversion
  3. temperatureThe mixture was cooled
  4. extractionthe mixture was extracted several times with ethyl acetate
  5. washThe combined ethyl acetate layers were washed with brine
  6. dry with materialdried over magnesium sulphate
  7. customevaporated