反应详情

To an aqueous solution of 2 mol/L NaOH (86 ml) was added dropwise under ice cooling a solution of 30.2 g of the compound obtained in Step 14-1 in MeOH (181 ml) under stirring over 60 minute, then the reaction mixture was stirred at room temperature for 16 hours. MeOH was evaporated under reduced pressure, to the solution was added toluene and stirred, then the aqueous layer was separated and the solution was stirred under ice cooling. To the solution was added dropwise 2 mol/L hydrochloric acid over 40 minutes, then extracted with EtOAc, the combined organic layer was washed with saturated brine, dried over Na2SO4, then, the drying agent was separated by filtration, and the solvent was evaporated under reduced pressure to obtain 25.1 g of a colorless solid. IPE (91 ml) was added, the suspension was stirred for 2 hours at room temperature, then, crystals were collected by filtration as 20.2 g of the title compound (colorless solid). The filtrate was concentrated under reduced pressure, IPE (9 ml) was added, stirred for 2 hours at room temperature, then, crystals were collected by filtration to 540 mg of the title compound (colorless solid).

1. stirringthe reaction mixture was stirred at room temperature for 16 hours
2. customMeOH was evaporated under reduced pressure, to the solution
3. additionwas added toluene
4. stirringstirred
5. customthe aqueous layer was separated
6. stirringthe solution was stirred under ice cooling
7. additionTo the solution was added dropwise 2 mol/L hydrochloric acid over 40 minutes
8. extractionextracted with EtOAc
9. washthe combined organic layer was washed with saturated brine
10. dry with materialdried over Na2SO4
11. customthe drying agent was separated by filtration
12. customthe solvent was evaporated under reduced pressure