تفاعل #75123

معادلة التفاعل

1-chloro-4-methyl-2-nitrobenzene

3-amino-1-propanol

→

3-[(4-methyl-2-nitrophenyl)amino]-1-propanol

المردود 33.0%

المذيبات

butanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for 30 hours
2. 2
   أخرىThe reaction mixture is evaporated
3. 3
   workup.ADDITIONthe residue is poured onto water
4. 4
   استخلاصThe product is extracted with methylbenzene
5. 5
   غسيلThe extract is washed with water and with a hydrochloric acid solution 2 N
6. 6
   أخرىdried
7. 7
   ترشيحfiltered
8. 8
   أخرىevaporated
9. 9
   أخرىThe residue is purified by column-chromatography over silica gel using
10. 10
    workup.ADDITIONa mixture of trichloromethane and 5% of methanol as eluent
11. 11
    أخرىThe pure fractions are collected
12. 12
    أخرىthe eluent is evaporated

الإجراء التجريبي

A mixture of 171 parts of 1-chloro-4-methyl-2-nitrobenzene, 150 parts of 3-amino-1-propanol and 400 parts of butanol is stirred and refluxed for 30 hours. The reaction mixture is evaporated and the residue is poured onto water. The product is extracted with methylbenzene. The extract is washed with water and with a hydrochloric acid solution 2 N, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 70 parts (33%) of 3-[(4-methyl-2-nitrophenyl)amino]-1-propanol as a residue.

المصدر