반응 #167778

반응 방정식

compound 101

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

ethyl acetate

→

title compound

수율 101.3%

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

수율 101.3%

용매

acetic acid

반응 조건

후처리

1. 1
   여과The reaction mixture was filtered by a glass
2. 2
   여과filter
3. 3
   세척the residue was washed with ethyl acetate (50 ml)
4. 4
   세척the mixture was successively washed with saturated aqueous ammonium chloride solution and brine
5. 5
   건조dried over sodium sulfate
6. 6
   농축concentrated
7. 7
   기타The residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1)

실험 절차

To the compound 101 (2.76 g) in an ethyl acetate (32 ml) and acetic acid (16 ml) suspension, zinc powder (2.88 g) was added under ice cooling, and the mixture was stirred at that temperature for 20 minutes and at room temperature for 4 hours. The reaction mixture was filtered by a glass filter spread with Celite®, then the residue was washed with ethyl acetate (50 ml). The filtrate and the washings were combined, then the mixture was successively washed with saturated aqueous ammonium chloride solution and brine, dried over sodium sulfate, then concentrated. The residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1) to obtain the title compound (2.5 g).

출처