반응 #2835

반응 방정식

dimethylformamide

1-hydroxybenzotriazole

N,N'-dicyclohexylcarbodiimide

morpholine

→

oil

2-valeramidoisonicotinic acid morpholide

반응 조건

후처리

1. 1
   기타The compound ([9]-(94)-467') (2.4610 g) prepared in Example 98
2. 2
   여과The insolubles were filtered out
3. 3
   농축the filtrate was concentrated
4. 4
   workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
5. 5
   세척washed with water and saturated brine
6. 6
   건조dried over anhydrous sodium sulfate
7. 7
   농축concentrated

실험 절차

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.

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