تفاعل #2419

معادلة التفاعل

acetone

oleum

4,4'-diamino-6-carbamoyl benzanilide

NH4OH

→

4,4'-diamino-6-cyanobenzanilide

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةalready cooled down to -5° to 0° C
2. 2
   غسيلThe solution was sufficiently washed
3. 3
   أخرىto remove salt
4. 4
   ترشيحby filtering
5. 5
   غسيلwashed with a small amount of warm ethanol
6. 6
   أخرىdried in a vacuum oven at 80° C
7. 7
   workup.ADDITIONThe dried reactant which was mixed with by-products
8. 8
   استخلاصwas extracted by soxlet
9. 9
   workup.ADDITIONtreated with the activated carbon
10. 10
    workup.ADDITIONethanol was added
11. 11
    أخرىto recrystallize in the mixture solvent (acetone:ethanol=1:1)
12. 12
    ترشيحThe light yellow-scalelike crystal was filtered
13. 13
    أخرىdried in a vacuum oven at 80° C
14. 14
    استخلاصThe light yellow-scalelike crystal was extracted again by soxlet with acetone
15. 15
    workup.ADDITIONtreated with the activated carbon
16. 16
    أخرىAnd then the white-scalelike crystal obtained
17. 17
    تجفيفwas dried in a vacuum oven at 80° C. (40 g of the raw material
18. 18
    أخرىwas obtained
19. 19
    أخرىthereof was 250° to 251° C.

الإجراء التجريبي

350 ml of oleum (30% by weight) was cooled down below 0° C. using an ice bath, 99.6 g (0.368 mol) of 4,4'-diamino-6-carbamoyl benzanilide in a powder form was added below 5° C. with stirring. The stirring was continued to the next day, and the solution was neutralized by adding 1100 ml of NH4OH (28% by weight) already cooled down to -5° to 0° C. The solution was sufficiently washed to remove salt by filtering and washed with a small amount of warm ethanol and then dried in a vacuum oven at 80° C. The dried reactant which was mixed with by-products was extracted by soxlet and treated with the activated carbon and then ethanol was added to recrystallize in the mixture solvent (acetone:ethanol=1:1). The light yellow-scalelike crystal was filtered and dried in a vacuum oven at 80° C. The light yellow-scalelike crystal was extracted again by soxlet with acetone and treated with the activated carbon. And then the white-scalelike crystal obtained by recrystalling in the mixture solvent (acetone:ethanol=1:1) was dried in a vacuum oven at 80° C. (40 g of the raw material was obtained and the boiling point thereof was 250° to 251° C.).

المصدر