HRID1248402
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
A stirred mixture of 5.0 g of 3-(4-piperidinyl)-1,2-benzisothiazole, 2.30 g of cyclopropylmethyl chloride, 7.95 g of potassium carbonate, 0.25 g of potassium iodide and 90 ml of dimethylformamide was heated at 90° for 20 hrs. The reaction mixture was poured into water and extracted with ethyl acetate. The organic extract was dried over anhydrous magnesium sulfate and the solvent was removed in vacuo to yield an oil. The oil was dissolved in ether and saturated hydrogen bromide/ether solution was added dropwise to precipitate the salt. The salt was recrystallized two times from ethyl acetate/ethanol to yield 2.0 g (25%) of product, mp 214°-216°.
WORKUP
后处理
- temperaturewas heated at 90° for 20 hrs
- extractionextracted with ethyl acetate
- extractionThe organic extract
- dry with materialwas dried over anhydrous magnesium sulfate
- customthe solvent was removed in vacuo
- customto yield an oil
- customto precipitate the salt
- customThe salt was recrystallized two times from ethyl acetate/ethanol