HRID52648

反应详情

EQUATION

反应方程式

HRID 52648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 10.0 grams (0.048 mole) of 6-chloro-7-cyano-2,3-dihydro-2,2-dimethylbenzofuran in 200 mL of 2-methyl-2-propanol was warmed to reflux, and 9.5 grams (0.17 mole) of 85% potassium hydroxide was added in one portion. Upon completion of addition, the reaction mixture was heated at reflux for about 75 minutes. The reaction mixture was then cooled and poured into 400 mL of water that was cooled in an ice bath. The resultant solid was collected by filtration and dried under vacuum, yielding 8.2 grams of 7-aminocarbonyl-6-chloro-2,3-dihydro-2,2-dimethylbenzofuran. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. temperatureto reflux
  2. additionUpon completion of addition
  3. temperaturethe reaction mixture was heated
  4. temperatureat reflux for about 75 minutes
  5. temperatureThe reaction mixture was then cooled
  6. temperaturewas cooled in an ice bath
  7. filtrationThe resultant solid was collected by filtration
  8. customdried under vacuum