反应详情

Under N2, to a solution of tert-butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenylcarbamate (500 mg, 1.57 mmol) in anhydrous THF (4 mL), was slowly added sodium hydride (94 mg, 2.35 mmol) at 0° C. The mixture was stirred at room temperature for 20 minutes, then cooled to 0° C. CH3I (445 mg, 3.13 mmol) was slowly added. After the completion of the addition, the reaction mixture was stirred at room temperature overnight, quenched with H2O, and extracted with EtOAc. The combined extracts were concentrated, and the residue was purified by flash chromatography to give the title compound. MS (m/z): 278 (M−56)+.

1. customat 0° C
2. temperaturecooled to 0° C
3. additionAfter the completion of the addition
4. stirringthe reaction mixture was stirred at room temperature overnight
5. customquenched with H2O
6. extractionextracted with EtOAc
7. concentrationThe combined extracts were concentrated
8. customthe residue was purified by flash chromatography