تفاعل #1760252

معادلة التفاعل

SnCl2.2H2O

hydrochloric acid

3,3′-dinitrobenzidine

→

3,3′-diaminobenzidine

المردود 74.0%

ظروف التفاعل

المعالجة

1. 1
   أخرىA 50 ml single neck round bottomed flask equipped with condenser
2. 2
   workup.ADDITIONwas added in small portions over 15 minute
3. 3
   درجة الحرارةto maintain the reaction temperature less than 60° C
4. 4
   workup.STIRRINGThe thick slurry was then stirred for additional 2 hours at 40° C.
5. 5
   أخرىThe salt of the tetramine was precipitated out
6. 6
   ترشيحthe solid filtered out
7. 7
   غسيلwashed with water
8. 8
   أخرىdried under vacuum

الإجراء التجريبي

A 50 ml single neck round bottomed flask equipped with condenser, and stirring magnetic bar were placed SnCl2.2H2O (12 g, 53 mmol) and 25 ml concentrated hydrochloric acid and reaction mixture was stirred and than 3,3′-dinitrobenzidine (DNB) of formula 2 where in R═H (2.16 g, 7.9 mmol) was added in small portions over 15 minute to maintain the reaction temperature less than 60° C. The thick slurry was then stirred for additional 2 hours at 40° C. to complete the reduction. The salt of the tetramine was precipitated out, which was neutralized with cold 10% NaOH solution and the solid filtered out, washed with water dried under vacuum to give 3,3′-diaminobenzidine (DAB) in 74% yield (1.26 g).

المصدر