反应详情

Trifluoroacetic acid (13.0 ml) is added to a solution of 1-((1,1-dimethylethoxy)-carbonyl-4-(N-methyl-N-(3-nitro-2-pyridinyl)amino)piperidine (PREPARATION 49) in methylene chloride (100 ml) with cooling to -78°. The mixture is warmed to 20°-25° , stirred 17 hrs, cooled to 0° and basified to pH 12 with 5% sodium hydroxide. The phases are separated and the aqueous phase is extracted with methylene chloride (2×50 ml). The combined organic phases are dried over sodium sulfate and concentrated to give the title compound, mp 115.5°-117°.

1. temperaturewith cooling to -78°
2. temperatureThe mixture is warmed to 20°-25°
3. customThe phases are separated
4. extractionthe aqueous phase is extracted with methylene chloride (2×50 ml)
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. concentrationconcentrated