反应 #2328981

反应方程式

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

NMP

trans-4-nitrocinnamoyl chloride

→

title compound

收率 78.1%

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

收率 78.1%

反应条件

后处理

1. 1
   其他purge
2. 2
   其他Thereafter, the ice bath was removed
3. 3
   workup.ADDITION400 mL of water was poured into the flask
4. 4
   其他to result in the formation of a solid precipitate, which
5. 5
   过滤was collected by filtration
6. 6
   workup.ADDITIONThe thus-obtained solid was added into 400 mL of water
7. 7
   温度heated to 60° C. for 10 min
8. 8
   过滤After filtration
9. 9
   过滤followed by filtration
10. 10
    其他An orange solid was obtained
11. 11
    其他dried in a vacuum oven at 80° C.

实验过程

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%.

来源