반응 #2832

반응 방정식

3-nitrobenzoic acid

1-hydroxybenzotriazole

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

morpholine

→

compound ( [13]-(132)-158 )

수율 89.8%

3-nitrobenzoic acid morpholide

수율 89.8%

용매

tetrahydrofuran

dichloromethane

chloroform

반응 조건

후처리

1. 1
   세척The mixture was washed with 1N-HCl aqueous solution, 1N-NaOH aqueous solution
2. 2
   workup.DISTILLATIONdistilled water
3. 3
   건조The organic layer was dried over anhydrous sodium sulfate
4. 4
   기타The solvent was evaporated under reduced pressure
5. 5
   기타the residue was purified by silica gel column chromatography (Kieselgel 60=160 g, ethyl acetate)

실험 절차

In tetrahydrofuran (100 ml) and dichloromethane (100 ml), 3-nitrobenzoic acid (7.58 g) was dissolved. Then 1-hydroxybenzotriazole (6.74 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (9.57 g), and morpholine (9.47 g) were added to the solution. The mixture was stirred at room temperature overnight. After the reaction was completed, chloroform was added to the solution. The mixture was washed with 1N-HCl aqueous solution, 1N-NaOH aqueous solution, and distilled water. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=160 g, ethyl acetate) to obtain the above-captioned compound ([13]-(132)-158) (9.62 g) as white crystals.

출처