反应详情

HATU (464 mg, 1.22 mmol, 1.0 equiv.) and DIPEA (0.8 ml, 4.88 mmol, 4.0 equiv.) were added at 0° C. to a suspension of 2-(7-((tert-butoxycarbonylamino)methyl)-1H-indol-1-yl)acetic acid (372 mg, 1.22 mmol, 1.0 equiv.) in THF (8 ml), and the mixture was stirred for 15 min. A solution of 3-pyridin-4-yl-3,9-diazaspiro[5.5]undecane (F-14) (283 mg, 1.22 mmol, 1.0 equiv.), dissolved in a mixture of THF (4 ml) and DMF (0.5 ml), was added, and stirring was carried out for 14 h at RT. The reaction mixture was diluted with ethyl acetate (30 ml) and extracted with sodium bicarbonate solution (2×20 ml), NH4Cl solution (2×20 ml), water (20 ml) and sat. NaCl solution (20 ml) and dried over Na2SO4. The solvent was removed under vacuum and the crude product was purified by column chromatography (Alox neutral; 0.5% MeOH/DCM), and the desired product was thus obtained in the form of a white solid.

1. additionwas added
2. stirringstirring
3. waitwas carried out for 14 h at RT
4. extractionextracted with sodium bicarbonate solution (2×20 ml), NH4Cl solution (2×20 ml), water (20 ml) and sat. NaCl solution (20 ml)
5. dry with materialdried over Na2SO4
6. customThe solvent was removed under vacuum
7. customthe crude product was purified by column chromatography (Alox neutral; 0.5% MeOH/DCM)