反応 #2823

反応方程式

Morpholine

3-nitro-4-valeramidobenzoic acid

Dicyclohexylcarbodiimide

1-hydroxybenzotriazole

→

3-nitro-4-valeramidobenzoic acid morpholide

溶媒

tetrahydrofuran

反応条件

後処理

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

実験手順

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.

出典