反应详情

温度

100 °C

5-tert-Butyl 3-ethyl 2-amino-6,7-dihydrothieno[3,2-c]pyridine-3,5(4H)-dicarboxylate from Example 73A (780 mg, 2.39 mmol) was dissolved in DMF (8 mL), and formamidine acetate (373 mg, 3.58 mmol) was added. The reaction mixture was heated to 100° C. overnight. The solvent was then removed in vacuo, and the residue was dissolved in ethyl acetate. The organic layer was washed 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 414 mg (56%) of the title compound as a tan solid. The mother liquor was concentrated and purified by preparative HPLC to yield a second batch of 36 mg (5%).

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