تفاعل #2063063

معادلة التفاعل

5-(methylamino)pentanol

2-chlorobenzothiazole

iodide

→

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

المردود 97.3%

المذيبات

methylisobutyl-keton

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed overnight
2. 2
   درجة الحرارةThe reaction mixture was cooled
3. 3
   غسيلwashed with water
4. 4
   أخرىdried
5. 5
   ترشيحfiltered
6. 6
   أخرىthe filtrate was evaporated
7. 7
   workup.STIRRINGThe residue was stirred in water
8. 8
   workup.STIRRINGstirred
9. 9
   غسيلwashed with diisopropylether
10. 10
    استخلاصThis mixture was extracted twice with CH2Cl2
11. 11
    أخرىThe separated organic layer was dried
12. 12
    ترشيحfiltered
13. 13
    أخرىthe solvent was evaporated

الإجراء التجريبي

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).

المصدر