反应详情

温度

50 °C

To a solution of 288 (0.350 g, 0.750 mmol) and MeOH:THF (6 mL, 1:1) was added hydrazine monohydrate (0.188 mL, 3.75 mmol) and the reaction was heated to 50° C. for 4 d. The reaction was then poured into water, and extracted with DCM. The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with DCM/MeOH (500:20) to afford 0.150 g (59.4%) of (R)-tert-butyl 3-amino-3-(3-fluoro-4-(trifluoromethyl)phenyl)propylcarbamate (290).

1. extractionextracted with DCM
2. dry with materialThe combined organic extracts were dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude product was purified by SiO2 chromatography
6. washeluting with DCM/MeOH (500:20)