反应详情

温度

-10 °C

To a 500 mL flask were added nitrile 2 (10.0 g, 30.95 mmol) and CH2Cl2 (130 mL). The solution was cooled to −10° C. and H2SO4 (10 mL) was added dropwise over 15 min. The mixture was stirred for 2 h at 0° C. Ice (200 g) was added and the mixture was stirred for 1 h. The mixture was basified with 32% aq NH3 to pH 8-9, EtOAc (400 mL) was added and the phases were separated. The aqueous phase was extracted with EtOAc (2×250 mL). The combined organic phases were dried over MgSO4 and were concentrated to provide 3 (11.1 g (9.99 g theoretical, the sample contains 10% w/w of EtOAc by NMR) 94%, 92.9% chemical purity, 97% de by HPLC/MS) as a white solid. HPLC/MS tR=3.04 min; m/z=342.1 (M+1)

1. stirringthe mixture was stirred for 1 h
2. additionwas added
3. customthe phases were separated
4. extractionThe aqueous phase was extracted with EtOAc (2×250 mL)
5. dry with materialThe combined organic phases were dried over MgSO4
6. concentrationwere concentrated
7. customto provide 3 (11.1 g (9.99 g theoretical