反应 #2823

反应方程式

Morpholine

3-nitro-4-valeramidobenzoic acid

Dicyclohexylcarbodiimide

1-hydroxybenzotriazole

→

3-nitro-4-valeramidobenzoic acid morpholide

溶剂

tetrahydrofuran

反应条件

后处理

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

实验过程

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.

来源