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
0.59 gram (5.17 millimoles) of mesyl chloride was added neat and in a dropwise manner over a 5 minute period to a stirred solution of 1.00 gram (3.62 millimoles) of 4-(5H-dibenzo[a,d]cyclohepten-5-yl)-piperidine and 1.45 grams (14.35 millimoles) of triethylamine in 10 milliliters of methylene chloride. The resulting solution was stirred an additional one-half hour and then diluted with 100 milliliters of methylene chloride. Thereafter the solution was washed with saturated sodium bicarbonate solution, then with brine and dried over magnesium sulfate. The drying agent was filtered off and the solvent vaporized in vacuo to obtain the desired 4-(5H-dibenzo[a,d]cyclohepten-5-yl)-1-(methylsulfonyl)piperidine product as a yellow solid residue. The product after recrystallization from ethyl acetate had a melting point of 260°-268° C. and elemental analyses as follows:
WORKUP
后处理
- washThereafter the solution was washed with saturated sodium bicarbonate solution
- dry with materialwith brine and dried over magnesium sulfate
- filtrationThe drying agent was filtered off