تفاعل #55049

معادلة التفاعل

2-bromopropane

4-(methoxymethyl)-N-phenyl-4-piperidinamine

N,N-diethylethanamine

→

4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine

المردود 42.6%

المذيبات

N,N-dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for 10.25 hours
2. 2
   درجة الحرارةAfter cooling
3. 3
   ترشيحthe formed N,N-diethylethanamine hydrobromide is filtered off
4. 4
   workup.ADDITIONthe filtrate is diluted with water
5. 5
   استخلاصThe product is extracted with methylbenzene
6. 6
   غسيلThe extract is washed thoroughly with water
7. 7
   أخرىdried
8. 8
   ترشيحfiltered
9. 9
   أخرىevaporated
10. 10
    أخرىThe residue is purified by column-chromatography over silica gel using
11. 11
    workup.ADDITIONa mixture of trichloromethane and methanol (90:10) as eluent
12. 12
    أخرىThe pure fractions are collected
13. 13
    أخرىthe eluent is evaporated

الإجراء التجريبي

A mixture of 10 parts of 2-bromopropane, 9 parts of 4-(methoxymethyl)-N-phenyl-4-piperidinamine, 4.9 parts of N,N-diethylethanamine and 72 parts of N,N-dimethylacetamide is stirred and refluxed for 10.25 hours. After cooling, the formed N,N-diethylethanamine hydrobromide is filtered off and the filtrate is diluted with water. The product is extracted with methylbenzene. The extract is washed thoroughly with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 5.7 parts (42.6%) of 4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine as an oily residue.

المصدر