反应详情

温度

80 °C

To a solution of ethyl 4-[(3-chloro-4-fluorophenyl)amino]-5,7-dihydro-6H-pyrrolo[3′,4′:4,5]thieno[2,3-d]pyrimidine-6-carboxylate from Example 22A (413 mg, 1.05 mmol) in ethanol (4 mL) was added a 10 M aqueous potassium hydroxide solution (2 mL), and the mixture was stirred for 14 h at 80° C. Subsequently, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed twice with water, dried over sodium sulfate, and the solvent was removed in vacuo. The residue was triturated with tert-butyl methyl ether, and the precipitate was collected by suction filtration to yield 126 mg (38%) of the title compound. The mother liquor was concentrated in vacuo and purified by preparative HPLC to yield further 35 mg (10%).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed twice with water
3. dry with materialdried over sodium sulfate
4. customthe solvent was removed in vacuo
5. customThe residue was triturated with tert-butyl methyl ether
6. filtrationthe precipitate was collected by suction filtration