HRID845437

反应详情

EQUATION

反应方程式

HRID 845437 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washThereafter the solution was washed with saturated sodium bicarbonate solution
  2. dry with materialwith brine and dried over magnesium sulfate
  3. filtrationThe drying agent was filtered off