反应 #1885095

反应方程式

N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide

potassium iodide

sodium carbonate

5-iodo-2-methyl-aniline

→

product

收率 96.9%

1-(5-Iodo-2-methyl-phenyl)-4-(toluene-4-sulfonyl)-piperazine

收率 96.9%

溶剂

cyclohexanol

反应条件

后处理

1. 1
   过滤At room temperature, the mixture was filtered
2. 2
   洗涤washed with dichloromethane
3. 3
   其他the filtrate evaporated to dryness
4. 4
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane
5. 5
   过滤filtered
6. 6
   其他the solvent evaporated
7. 7
   过滤the crystalline product filtered off
8. 8
   洗涤washed several times with n-heptane
9. 9
   其他dried in vacuo

实验过程

9.97 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide (30.3 mmol) and 5.03 g of potassium iodide (30.3 mmol) in 75 mL of cyclohexanol were stirred for 1 h at 80° C. After addition of 7.7 g of sodium carbonate (72.7 mmol) and 5.65 g of 5-iodo-2-methyl-aniline (24.2 mmol), stirring continued for 8 h at 160° C. At room temperature, the mixture was filtered, washed with dichloromethane, and the filtrate evaporated to dryness. The residue was dissolved in dichloromethane, filtered, and the solvent evaporated. The remaining residue was trituated with n-heptane and the crystalline product filtered off, washed several times with n-heptane and dried in vacuo to yield 10.7 g of product.

来源