反应详情

A mixture of tBuOH (10 mL), H2O (10 mL), ACN (1.8 mL) and ADmix-α (1.28 g) was stirred for 5 min at room temperature and then cooled to 0° C. at which time 1-(4-methoxybenzyl)-6-vinyl-1H-indazole (320 mg, 1.21 mmol) was added. The reaction was stirred for 18 h and allowed to warm to room temperature. The reaction was then diluted with H2O (25 mL) and extracted 3× with CH2Cl2. The organic layer was separated, washed with brine, dried over MgSO4 and the solvent removed to give a white solid which was sonicated with hexane/Et2O (1:1) and then filtered to give the title compound (270 mg, 75% after drying); 1H NMR (400 MHz, CD3OD) δ 8.01 (s, 1H), 7.72 (d, J=8.2 Hz, 1H), 7.58 (s, 1H), 7.19-7.13 (m, 3H), 6.82 (d, J=8.4 Hz, 2H), 5.56 (s, 2H), 4.82-4.79 (m, 1H), 3.73 (s, 3H), 3.69-3.59 (m, 2H); MS ESI 298.9 [M+H]+, calcd for [C17H18N2O3+H]+ 299.14.

1. additionwas added
2. stirringThe reaction was stirred for 18 h
3. temperatureto warm to room temperature
4. extractionextracted 3× with CH2Cl2
5. customThe organic layer was separated
6. washwashed with brine
7. dry with materialdried over MgSO4
8. customthe solvent removed
9. customto give a white solid which
10. filtrationfiltered