反应 #167778

反应方程式

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

收率 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

收率 101.3%

溶剂

acetic acid

反应条件

后处理

1. 1
   过滤The reaction mixture was filtered by a glass
2. 2
   过滤filter
3. 3
   洗涤the residue was washed with ethyl acetate (50 ml)
4. 4
   洗涤the mixture was successively washed with saturated aqueous ammonium chloride solution and brine
5. 5
   干燥dried over sodium sulfate
6. 6
   浓缩concentrated
7. 7
   其他The residue was purified by flash column chromatography (silica gel, hexane/ethyl acetate/methanol=6/6/1)

实验过程

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).

来源