反応 #2419

反応方程式

acetone

oleum

4,4'-diamino-6-carbamoyl benzanilide

NH4OH

→

4,4'-diamino-6-cyanobenzanilide

溶媒

ethanol

反応条件

後処理

1. 1
   温度already cooled down to -5° to 0° C
2. 2
   洗浄The solution was sufficiently washed
3. 3
   その他to remove salt
4. 4
   ろ過by filtering
5. 5
   洗浄washed with a small amount of warm ethanol
6. 6
   その他dried in a vacuum oven at 80° C
7. 7
   workup.ADDITIONThe dried reactant which was mixed with by-products
8. 8
   抽出was extracted by soxlet
9. 9
   workup.ADDITIONtreated with the activated carbon
10. 10
    workup.ADDITIONethanol was added
11. 11
    その他to recrystallize in the mixture solvent (acetone:ethanol=1:1)
12. 12
    ろ過The light yellow-scalelike crystal was filtered
13. 13
    その他dried in a vacuum oven at 80° C
14. 14
    抽出The light yellow-scalelike crystal was extracted again by soxlet with acetone
15. 15
    workup.ADDITIONtreated with the activated carbon
16. 16
    その他And then the white-scalelike crystal obtained
17. 17
    乾燥was dried in a vacuum oven at 80° C. (40 g of the raw material
18. 18
    その他was obtained
19. 19
    その他thereof was 250° to 251° C.

実験手順

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.).

出典