تفاعل #2823

معادلة التفاعل

Morpholine

3-nitro-4-valeramidobenzoic acid

Dicyclohexylcarbodiimide

1-hydroxybenzotriazole

→

3-nitro-4-valeramidobenzoic acid morpholide

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGThe mixture was stirred for 16 hours
2. 2
   أخرىAfter the insolubles were removed from the reaction solution
3. 3
   تركيزthe solution was concentrated
4. 4
   أخرىdried
5. 5
   workup.DISSOLUTIONThe crude product was dissolved in chloroform
6. 6
   أخرىthe insolubles were removed
7. 7
   أخرىthe solution was purified by silica gel column chromatography (Kieselgel 60=400 g, chloroform/methanol=30/1)
8. 8
   أخرىto obtain the compound ([1]-(12)-1) (22.95 g) as yellow needle crystals

الإجراء التجريبي

In tetrahydrofuran (800 ml), 3-nitro-4-valeramidobenzoic acid ([1]-(11)-1) (20.0 g) was dissolved. Dicyclohexylcarbodiimide (17.1 g) and 1-hydroxybenzotriazole (11.2 g) were added to the solution, and the mixture was stirred at room temperature for 15 minutes. Morpholine (7.27 g) was further added to the solution. The mixture was stirred for 16 hours. After the insolubles were removed from the reaction solution, the solution was concentrated and dried. The crude product was dissolved in chloroform, and the insolubles were removed, and the solution was purified by silica gel column chromatography (Kieselgel 60=400 g, chloroform/methanol=30/1) to obtain the compound ([1]-(12)-1) (22.95 g) as yellow needle crystals.

المصدر