反应详情

To a solution of compound 1c (8.40 g, 30.4 mmol) in THF (100 mL) was added LiAlH4 (2.55 g, 60.8 mmol) in portions at 0° C. The reaction mixture was stirred at rt for 2 h. The reaction was slowly quenched with H2O (10 mL). The resulting mixture was extracted with DCM (2×100 mL), and the combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to obtain compound 1d as a yellow solid (3.80 g, 53% yield). Mass Spectrum (LCMS, ESI pos.): Calcd. for C11H14N4O2: 235.1 (M+H). found: 235.2.

1. customThe reaction was slowly quenched with H2O (10 mL)
2. extractionThe resulting mixture was extracted with DCM (2×100 mL)
3. washthe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure