Reaktion #2835

Reaktionsgleichung

dimethylformamide

1-hydroxybenzotriazole

N,N'-dicyclohexylcarbodiimide

morpholine

→

oil

2-valeramidoisonicotinic acid morpholide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe compound ([9]-(94)-467') (2.4610 g) prepared in Example 98
2. 2
   FiltrationThe insolubles were filtered out
3. 3
   Einengenthe filtrate was concentrated
4. 4
   workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
5. 5
   Waschenwashed with water and saturated brine
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   Einengenconcentrated

Vorschrift

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.

Quelle