反应详情

温度

-78 °C

To a solution of (6-formyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-carbamic acid tert-butyl ester (Step c, 2.80 g, 10.2 mmol, 1.0 eq) in THF (100 mL) at −78° C. was added a solution of MeMgBr (Aldrich, 1.4 M in toluene/THF (3:1), 29 mL, 40.7 mmol, 4.0 eq) slowly. The reaction was stirred at −78° C. for 20 min, warmed to RT and stirred at RT for 2 h. The reaction was quenched with saturated NaHCO3 (120 mL), and the crude was extracted with EtOAc (100 mL×3). The extract phase was washed with saturated NaCl, dried over Na2SO4, filtered and concentrated. The title compound was obtained as a white solid. MS (ESI, pos. ion) m/z: 292 (M+1).

1. temperaturewarmed to RT
2. stirringstirred at RT for 2 h
3. customThe reaction was quenched with saturated NaHCO3 (120 mL)
4. extractionthe crude was extracted with EtOAc (100 mL×3)
5. washThe extract phase was washed with saturated NaCl
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated