反应详情

温度

80 °C

To a solution of compound 2b (5.00 g, 10.9 mmol, as prepared in Example 2, Step B) in DME/H2O (10:1 v/v, 150 mL) was added TosNHNH2 (6.41 g, 34.5 mmol) and NaOAc (4.70 g, 57.3 mmol). The reaction mixture was stirred at 80° C. overnight. After cooling to rt, the reaction was quenched with H2O (200 mL). The solids were collected by filtration and washed with Et2O to obtain compound 3a as a white solid (3.50 g, 67% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C21H20BrN5O: 438.1 (M+H). found: 438.1.

1. temperatureAfter cooling to rt
2. customthe reaction was quenched with H2O (200 mL)
3. filtrationThe solids were collected by filtration
4. washwashed with Et2O