HRID72852
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed overnight
- temperatureAfter cooling
- extractionthe mixture extracted
- additionA solution of NaOH was added to the aqueous phase until pH 11
- extractionthe mixture was extracted with ethyl acetate three times
- dry with materialThe combined ethyl acetate fractions were dried
- customevaporated under reduced pressure