반응 #167769

반응 방정식

compound 77a

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

hydrochloric acid

→

title compound

수율 161.7%

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

수율 161.7%

용매

acetic acid

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   농축The reaction solution was concentrated
3. 3
   workup.ADDITIONthe residue was diluted with ethyl acetate
4. 4
   workup.ADDITIONTo this solution, a 1M hydrochloric acid in acetic acid solution was added
5. 5
   workup.STIRRINGthe mixture was stirred
6. 6
   workup.ADDITIONFurther, diethyl ether was added
7. 7
   여과the precipitated solid was collected by filtration

실험 절차

To the compound 77a (523 mg) obtained at Step (1), 1M hydrochloric acid in acetic acid solution (18 ml) was added, and the mixture was stirred at room temperature for 2.5 hours. The reaction solution was concentrated, then the residue was diluted with ethyl acetate. To this solution, a 1M hydrochloric acid in acetic acid solution was added and the mixture was stirred. Further, diethyl ether was added, and the precipitated solid was collected by filtration to obtain the title compound (410 mg).

출처