تفاعل #2328982

معادلة التفاعل

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

4-hydroxybenzoic acid

→

title compound

المردود 76.3%

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

المردود 76.3%

المذيبات

NMP

ظروف التفاعل

المعالجة

1. 1
   أخرىpurge
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
   درجة الحرارةThe 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
   ترشيحthe resultant precipitate was collected by filtration
6. 6
   غسيلwashed with water (400 mL
7. 7
   أخرىby drying at room temperature under vacuum overnight

الإجراء التجريبي

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%.

المصدر