تفاعل #167778

معادلة التفاعل

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

المردود 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

المردود 101.3%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe reaction mixture was filtered by a glass
2. 2
   ترشيحfilter
3. 3
   غسيلthe residue was washed with ethyl acetate (50 ml)
4. 4
   غسيلthe mixture was successively washed with saturated aqueous ammonium chloride solution and brine
5. 5
   تجفيفdried over sodium sulfate
6. 6
   تركيزconcentrated
7. 7
   أخرىThe residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1)

الإجراء التجريبي

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).

المصدر