反应详情

A solution of 1,1-dimethylethyl 4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate (may be prepared as described in Description 9) (75 mg, 0.32 mmol), [4-(methylsulfonyl)phenyl]boronic acid (128 mg, 0.64 mmol), copper acetate (116 mg, 0.64 mmol), molecular sieves (4 Å, 0.2 g) and pyridine (52 μl, 0.64 mmol) in dichloromethane (2.5 ml) was stirred at room temperature open to atmosphere for 60 hours. The mixture was then diluted with methanol and filtered through a celite pad washing with methanol. The solvent was evaporated in vacuo. Residue was taken up into ethyl acetate and washed with water and 5% aq. sodium hydrogen carbonate, then dried over magnesium sulphate and evaporated in vacuo. The resulting residue was purified by MDAP to afford the title compound (D32). MS (ES+) m/e 392 [M+H]+.

1. filtrationfiltered through a celite pad
2. washwashing with methanol
3. customThe solvent was evaporated in vacuo
4. washwashed with water and 5% aq. sodium hydrogen carbonate
5. dry with materialdried over magnesium sulphate
6. customevaporated in vacuo
7. customThe resulting residue was purified by MDAP