HRID66823

反应详情

EQUATION

反应方程式

HRID 66823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

One hundred and forty-one grams (0.75 mole) of 2-(4-picolinylidene)1,3,4,5,6,7-hexahydroazepine were dissolved in 1000 ml of chloroform and mixed under ice cooling with a solution of 89 g (0.83 mole) of 1,4-benzoquinone in 1000 ml of chloroform added dropwise. After the mixture stood for 24 hours at room temperature, the precipitate formed was filtered, suspended in 500 ml of dimethylformamide, and then heated for two hours to 100° C. After cooling, the suspension was suction filtered and washed with dimethylformamide and acetone, whereby the pure 2-hydroxy-isomer was obtained.

WORKUP

后处理

  1. additionadded dropwise
  2. customthe precipitate formed
  3. filtrationwas filtered
  4. temperatureheated for two hours to 100° C
  5. temperatureAfter cooling
  6. filtrationfiltered
  7. washwashed with dimethylformamide and acetone, whereby the pure 2-hydroxy-isomer
  8. customwas obtained