반응 #2328982

반응 방정식

2,5-Bis[(2-cyanoethyl)sulfanyl]-N-(4-nitrobenzoyl)-1,4-phenylenediamine

4-hydroxybenzoic acid

→

title compound

수율 76.3%

2,5-bis[(2-cyanoethyl)sulfanyl]-N-(p-hydroxybenzoyl)-N′-(p-nitrobenzoyl)-p-phenylenediamine

수율 76.3%

용매

NMP

반응 조건

후처리

1. 1
   기타purge
2. 2
   workup.ADDITIONfollowed by addition of lithium chloride (LiCl, 0.58 g), triphenylphosphite (TPP, 2.92 mL) and pyridine (2.92 mL)
3. 3
   온도The resultant mixture was heated to a temperature of 80˜95° C. for about 4 h
4. 4
   workup.ADDITION400 mL of water was subsequently added
5. 5
   여과the resultant precipitate was collected by filtration
6. 6
   세척washed with water (400 mL
7. 7
   기타by drying at room temperature under vacuum overnight

실험 절차

2,5-Bis[(2-cyanoethyl)sulfanyl]-N-(4-nitrobenzoyl)-1,4-phenylenediamine (1.0 g, 2.34 mmol) as prepared from the above Example 1 was admixed with 4-hydroxybenzoic acid (0.328 g, 2.38 mmol) in 11.7 mL NMP under nitrogen purge, followed by addition of lithium chloride (LiCl, 0.58 g), triphenylphosphite (TPP, 2.92 mL) and pyridine (2.92 mL). The resultant mixture was heated to a temperature of 80˜95° C. for about 4 h, followed by cooling to room temperature. 400 mL of water was subsequently added with stirring for a few minutes, and the resultant precipitate was collected by filtration, washed with water (400 mL, twice) and methanol (400 mL, once), followed by drying at room temperature under vacuum overnight, giving the title compound in a yield of 76.3%.

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