반응 #2063063

반응 방정식

5-(methylamino)pentanol

2-chlorobenzothiazole

iodide

→

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

수율 97.3%

용매

methylisobutyl-keton

반응 조건

후처리

1. 1
   온도refluxed overnight
2. 2
   온도The reaction mixture was cooled
3. 3
   세척washed with water
4. 4
   기타dried
5. 5
   여과filtered
6. 6
   기타the filtrate was evaporated
7. 7
   workup.STIRRINGThe residue was stirred in water
8. 8
   workup.STIRRINGstirred
9. 9
   세척washed with diisopropylether
10. 10
    추출This mixture was extracted twice with CH2Cl2
11. 11
    기타The separated organic layer was dried
12. 12
    여과filtered
13. 13
    기타the solvent was evaporated

실험 절차

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).

출처