反应详情

A mixture of 1-cyano-4-hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid methyl ester (50 mg, 0.16 mmole) and 3-(aminomethyl)-5-methylhexanoic acid (249 mg, 1.6 mmole, AK Scientific) in 0.5 M sodium methoxide in methanol (2.5 ml) was refluxed for two days before it was cooled to room temperature, concentrated and dissolved in water, extracted with dichloromethane. The remaining aqueous layer was acidified with 1N hydrochloric chloride, extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, concentrated and purified by flash column chromatography on silica gel with a gradient of dichloromethane and ethyl acetate to give the title compound as a white solid (35 mg). LC-MS ESI+: 448 (M+1)+; ESI−: 446 (M-1)−.

1. temperaturewas refluxed for two days before it
2. concentrationconcentrated
3. dissolutiondissolved in water
4. extractionextracted with dichloromethane
5. extractionextracted with dichloromethane
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. concentrationconcentrated
8. custompurified by flash column chromatography on silica gel with a gradient of dichloromethane and ethyl acetate