反应 #2835

反应方程式

dimethylformamide

1-hydroxybenzotriazole

N,N'-dicyclohexylcarbodiimide

morpholine

→

oil

2-valeramidoisonicotinic acid morpholide

反应条件

后处理

1. 1
   其他The compound ([9]-(94)-467') (2.4610 g) prepared in Example 98
2. 2
   过滤The insolubles were filtered out
3. 3
   浓缩the filtrate was concentrated
4. 4
   workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
5. 5
   洗涤washed with water and saturated brine
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   浓缩concentrated

实验过程

The compound ([9]-(94)-467') (2.4610 g) prepared in Example 98 was dissolved in anhydrous dimethylformamide (DMF) (37 ml). Then, 1-hydroxybenzotriazole (1.9477 g), N,N'-dicyclohexylcarbodiimide (2.9739 g), and morpholine (1.3 ml) were added to the solution. The mixture was stirred at room temperature for 16 hours. The insolubles were filtered out, and the filtrate was concentrated. The resulting residue was dissolved in chloroform, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated to obtain yellowish brown oil (7.4981 g). The crude oil was purified by silica gel column chromatography (Kieselgel 60=230 g, chloroform/acetone=5/1) to obtain the above-captioned compound ([9]-(94)-467") (3.1756 g) as white crystals.

来源