反应详情

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 5-{3-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-phenyl}-oxazole-4-carboxylic acid (130 mg, 0.37 mmol) in CH2Cl2 (2.7 mL) was treated sequentially with DMAP (11 mg, 0.09 mmol), HOBt (60 mg, 0.45 mmol), EDC (179 mg, 0.94 mmol) and DIPEA (0.25 mL, 1.50 mmol) and the reaction mixture was stirred at rt for 1 h. A solution of 1-[5-(2-methyl-[1,3]dioxolan-2-yl)-furan-2-ylmethyl]-1H-pyrazol-3-ylamine (93 mg, 0.37 mmol) in CH2Cl2 (1.0 mL) was then added and the reaction mixture was stirred at rt for 48 h. CH2Cl2 (10 mL) was added followed by water (10 mL). The organic layer was dried over MgSO4, filtered, and the solvent removed under reduced pressure. Purification of the residue by FC (1:2 hept-EA) gave the title compound as a colorless oil. TLC: rf (1:2 hept-EA)=0.26. LC-MS-conditions 02: tR=1.22 min, [M+H]+=579.74.

1. stirringthe reaction mixture was stirred at rt for 48 h
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. customthe solvent removed under reduced pressure
5. customPurification of the residue by FC (1:2 hept-EA)