反应 #2063063

反应方程式

5-(methylamino)pentanol

2-chlorobenzothiazole

iodide

→

N-(5-hydroxypentyl)-N-methyl-2-benzothiazolamine

收率 97.3%

溶剂

methylisobutyl-keton

反应条件

后处理

1. 1
   温度refluxed overnight
2. 2
   温度The reaction mixture was cooled
3. 3
   洗涤washed with water
4. 4
   其他dried
5. 5
   过滤filtered
6. 6
   其他the filtrate was evaporated
7. 7
   workup.STIRRINGThe residue was stirred in water
8. 8
   workup.STIRRINGstirred
9. 9
   洗涤washed with diisopropylether
10. 10
    萃取This mixture was extracted twice with CH2Cl2
11. 11
    其他The separated organic layer was dried
12. 12
    过滤filtered
13. 13
    其他the solvent was evaporated

实验过程

A mixture of 5-(methylamino)pentanol (0.23 mol), 2-chlorobenzothiazole (0.3 mol), sodium carbonate (0.4 g) and potssium iodide (catalytic quantity) in methylisobutyl-keton (1000 ml) was stirred and refluxed overnight. The reaction mixture was cooled, washed with water, dried, filtered and the filtrate was evaporated. The residue was stirred in water, acidified with HCl, stirred, washed with diisopropylether, and the acidic layer was alkalized with NH4OH. This mixture was extracted twice with CH2Cl2. The separated organic layer was dried, filtered, and the solvent was evaporated, yielding 56 g of N-(5-hydroxypentyl)-N-methyl-2-benzothiazolamine (interm. 7).

来源