반응 #2328981

반응 방정식

2,5-Bis[(cyanoethyl)thio]-1,4-phenylenediamine

NMP

trans-4-nitrocinnamoyl chloride

→

title compound

수율 78.1%

N-{4-Amino-2,5-bis[(2-cyanoethyl)sulfanyl]-phenyl}-trans-4-nitrocinnamoyl formamide

수율 78.1%

반응 조건

후처리

1. 1
   기타purge
2. 2
   기타Thereafter, the ice bath was removed
3. 3
   workup.ADDITION400 mL of water was poured into the flask
4. 4
   기타to result in the formation of a solid precipitate, which
5. 5
   여과was collected by filtration
6. 6
   workup.ADDITIONThe thus-obtained solid was added into 400 mL of water
7. 7
   온도heated to 60° C. for 10 min
8. 8
   여과After filtration
9. 9
   여과followed by filtration
10. 10
    기타An orange solid was obtained
11. 11
    기타dried in a vacuum oven at 80° C.

실험 절차

2,5-Bis[(cyanoethyl)thio]-1,4-phenylenediamine (2.50 g, 9.00 mmol) was admixed with 15 mL of NMP in a 250 mL 3-necked round-bottom flask with nitrogen purge. The resultant mixture was cooled to around 0° C. in an ice bath with stirring, followed by the addition of trans-4-nitrocinnamoyl chloride (2.00 g, 9.45 mmol, dissolved in 13 mL NMP) drop by drop. Thereafter, the ice bath was removed, and 400 mL of water was poured into the flask to result in the formation of a solid precipitate, which was collected by filtration. The thus-obtained solid was added into 400 mL of water and heated to 60° C. for 10 min. After filtration, the collected solid was admixed with 600 mL of methanol, followed by filtration. An orange solid was obtained and dried in a vacuum oven at 80° C., giving the title compound in a yield of 78.13%.

출처