反应详情

11 g 3-oxo-2,3,5,6,8,9-hexahydro-1,2,7-triaza-benzocycloheptene-7-carboxylic acid tert-butyl ester in 90 ml phosphor oxychloride was refluxed overnight. The phosphor oxychloride was quenched with 8.7 g sodium carbonate to pH 8 and 100 mL water was added to the reaction mixture. Di-tert.butyl-dicarbonate was added to the reaction mixture and stirred over night. The solution was extracted with 50% ethyl acetate in hexane. The extracted organic layer was dried, concentrated under reduced pressure and purified by column chromatography to afford 8.0 g of the desired product. (M+H)+=284

1. customThe phosphor oxychloride was quenched with 8.7 g sodium carbonate to pH 8 and 100 mL water
2. additionwas added to the reaction mixture
3. additionDi-tert.butyl-dicarbonate was added to the reaction mixture
4. extractionThe solution was extracted with 50% ethyl acetate in hexane
5. customThe extracted organic layer was dried
6. concentrationconcentrated under reduced pressure
7. custompurified by column chromatography