反応 #2835

反応方程式

dimethylformamide

1-hydroxybenzotriazole

N,N'-dicyclohexylcarbodiimide

morpholine

→

oil

2-valeramidoisonicotinic acid morpholide

反応条件

後処理

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

実験手順

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.

出典