反应详情

{1-Benzyl-2-hydroxy-3-[isobutyl-(3-methyl-1H-indazole-5-sulfonyl)-amino]-propyl}-carbamic acid tert-butyl ester (25 mg, 0.047 mmol) was added to a solution of 4N HCl in dioxane (0.25 mL). Material precipitated out so 800 uL conc. HCl was added and the reaction heated at reflux for 2 h. The resulting solution was concentrated under vacuum and concentrated 2 additional times from 1 mL methylene chloride. This crude amine was dissolved in 0.5 mL methylene chloride and diisopropylethylamine (80 uL, 0.46 mmol) was then added. To this solution was added carbonic acid 2,5-dioxo-pyrrolidin-1-yl ester hexahydro-furo[2,3-b]furan-3-yl ester (16 mg, 0.055 mmol) and the reaction stirred overnight. The reaction was concentrated under vacuum and purified by preparative HPLC. MS 587 (MH+).

1. customMaterial precipitated out so 800 uL conc. HCl
2. additionwas added
3. temperaturethe reaction heated
4. temperatureat reflux for 2 h
5. concentrationThe resulting solution was concentrated under vacuum
6. concentrationconcentrated 2 additional times from 1 mL methylene chloride
7. dissolutionThis crude amine was dissolved in 0.5 mL methylene chloride
8. concentrationThe reaction was concentrated under vacuum
9. custompurified by preparative HPLC