HRID72852

反应详情

EQUATION

反应方程式

HRID 72852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[4-(6-Chloro-benzo[d]isoxazol-3-yl)-piperidin-1-yl]-ethanone (1.45 g, 5.3 mmol) was diluted with an aqueous solution of HCl 6N (13.8 mL, 16 mmol) and the mixture was refluxed overnight. After cooling, 2×20 mL of ether was added and the mixture extracted. A solution of NaOH was added to the aqueous phase until pH 11 and the mixture was extracted with ethyl acetate three times. The combined ethyl acetate fractions were dried and evaporated under reduced pressure to yield 1.14 g of a light brown solid (93%). MS (m/e): 236.9 (M+H+).

WORKUP

后处理

  1. temperaturethe mixture was refluxed overnight
  2. temperatureAfter cooling
  3. extractionthe mixture extracted
  4. additionA solution of NaOH was added to the aqueous phase until pH 11
  5. extractionthe mixture was extracted with ethyl acetate three times
  6. dry with materialThe combined ethyl acetate fractions were dried
  7. customevaporated under reduced pressure