تفاعل #5877

معادلة التفاعل

sodium hydroxide

methyl 1-(2,3-dihydro-3-methyl-1H-inden-1-yl)-2-mercapto-1H-imidazole-5-carboxylate

nitric acid

→

methyl 1-(2,3-dihydro-3-methyl-1H-inden-1-yl)-1H-imidazole-5-carboxylate mononitrate

المردود 62.6%

ظروف التفاعل

المعالجة

1. 1
   أخرى(intense reaction)
2. 2
   workup.ADDITIONThe reaction mixture is poured
3. 3
   أخرىinto crushed ice
4. 4
   استخلاصThe product is extracted with trichloromethane
5. 5
   غسيلThe extract is washed with water
6. 6
   أخرىdried
7. 7
   ترشيحfiltered
8. 8
   أخرىevaporated
9. 9
   ترشيحThe salt is filtered off
10. 10
    أخرىdried

الإجراء التجريبي

A mixture of 10 parts of methyl 1-(2,3-dihydro-3-methyl-1H-inden-1-yl)-2-mercapto-1H-imidazole-5-carboxylate and 120 parts of a nitric acid solution 30% is stirred for 30 minutes at room temperature (intense reaction). The reaction mixture is poured into crushed ice and treated with a sodium hydroxide solution. The product is extracted with trichloromethane. The extract is washed with water, dried, filtered and evaporated. The residue is converted into the nitrate salt in 2-propanone and 2,2'-oxybispropane. The salt is filtered off and dried, yielding 6.8 parts (62.6%) of methyl 1-(2,3-dihydro-3-methyl-1H-inden-1-yl)-1H-imidazole-5-carboxylate mononitrate; mp. 140.3° C. (compound 2.35).

المصدر