反応 #2063063

反応方程式

5-(methylamino)pentanol

2-chlorobenzothiazole

iodide

→

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

収率 97.3%

溶媒

methylisobutyl-keton

反応条件

後処理

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

実験手順

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).

出典