HRID128713

反应详情

EQUATION

反应方程式

HRID 128713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

112 mmol of potassium cyanide and 116 mmol of ammonium chloride ate added successively to a solution, maintained under nitrogen and with stirring, containing 110 mmol of 5-methoxy-3,4-dihydronaphthalen-2(1H)-one in 90 ml of ethanol and 50 ml of water. The whole mixture is stirred for 20 hours at 20° C. and then concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate. This phase is then washed with water and extracted with 1N hydrochloric acid. The acid phase is basified with 35% sodium hydroxide solution and extracted with methyl acetate. The combined organic phases are dried and evaporated under vacuum and lead to the expected product in the solid form.

WORKUP

后处理

  1. temperaturemaintained under nitrogen
  2. stirringThe whole mixture is stirred for 20 hours at 20° C.
  3. concentrationconcentrated under vacuum
  4. washThis phase is then washed with water
  5. extractionextracted with 1N hydrochloric acid
  6. extractionextracted with methyl acetate
  7. customThe combined organic phases are dried
  8. customevaporated under vacuum and lead to the expected product in the solid form