반응 #2830

반응 방정식

water

4-methoxycarbonylbenzaldehyde

compound ( [5]-(55)-75 )

3-amino-4-hexylbenzoic acid morpholide

→

4-hexyl-3-[(4-methoxycarbonylphenyl)methyl]aminobenzoic acid morpholide

용매

acetic acid

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was stirred at room temperature for 30 minutes
2. 2
   추출The solution was extracted with ethyl acetate
3. 3
   세척washed with distilled water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타The solvent was evaporated under reduced pressure
6. 6
   기타the residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1)
7. 7
   기타to obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid

실험 절차

The compound ([5]-(55)-75) (600 mg) prepared in Example 63 was dissolved in acetic acid (6.0 ml). Then, 4-methoxycarbonylbenzaldehyde (373 mg) was added. The mixture was stirred at room temperature for 4 hours. Then, boranediethylamine complex (146 mg) was added to the solution. The mixture was stirred at room temperature for 30 minutes. After the reaction was completed, water was added to the solution. The solution was extracted with ethyl acetate, washed with distilled water, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=30 g, hexane/ethyl acetate=1/1) to obtain the above-captioned compound ([5]-(57)-75') (841 mg) as a white solid.

출처