반응 #167762

반응 방정식

compound 54

(2R)-2-({[(6R)-6-(5-chloro-2-methoxybenzyl)-7-oxo-3-(phenoxyimino)-1,4-diazepan-1-yl]carbonyl}amino)butanoic acid

methylene chloride

dimethylamine

methanol

→

title compound

(6R)-6-(5-chloro-2-methoxybenzyl)-N-[(1R)-1-(methylcarbamoyl)propyl]-7-oxo-3-(phenoxyimino)-1,4-diazepane-1-carboxamide

용매

triethylamine

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent was distilled off
2. 2
   workup.ADDITIONthe residue was diluted with ethyl acetate
3. 3
   세척Then the resultant mixture was successively washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium hydrogencarbonate solution, and brine
4. 4
   건조The organic layer was dried over anhydrous sodium sulfate
5. 5
   농축was concentrated
6. 6
   기타The residue was purified by flash column chromatography (silica gel, chloroform/ethyl acetate=9/1 to 1/1)

실험 절차

To the compound 54 (70 mg) in a methylene chloride (3 ml) solution, dimethylamine in a methanol solution (2M, 0.14 ml), triethylamine (0.291 ml), and propyl phosphonate anhydride (T3P) (50% ethyl acetate solution, 0.21 ml) were successively added, and the mixture was stirred at room temperature for 30 minutes. The solvent was distilled off, and the residue was diluted with ethyl acetate. Then the resultant mixture was successively washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium hydrogencarbonate solution, and brine. The organic layer was dried over anhydrous sodium sulfate, then was concentrated. The residue was purified by flash column chromatography (silica gel, chloroform/ethyl acetate=9/1 to 1/1) to obtain the title compound (42.5 mg).

출처