반응 #2823

반응 방정식

Morpholine

3-nitro-4-valeramidobenzoic acid

Dicyclohexylcarbodiimide

1-hydroxybenzotriazole

→

3-nitro-4-valeramidobenzoic acid morpholide

용매

tetrahydrofuran

반응 조건

후처리

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

실험 절차

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.

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