反应详情

温度

135 °C

A mixture of 2-bromo-1-cyclobutylethanone (27.2 g, 154 mmol) and formamidine acetate (80.0 g, 768 mmol) in ethyleneglycol (150 mL) was heated to 135° C. for 18 h. The mixture was then diluted with H2O and then continuously extracted with Et2O for 18 h. The org. phase was then dried over Na2SO4, filtered and concentrated in vacuo. Purification by distillation in a Kugelrohr oven and flash chromatography (SiO2, DCM to DCM/MeOH 9:1) afforded the title compound (3.5 g). UPLC-MS: MS 123.1 (M+H+); UPLC rt 0.36 min.

1. extractioncontinuously extracted with Et2O for 18 h
2. dry with materialphase was then dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customPurification
6. distillationby distillation in a Kugelrohr oven and flash chromatography (SiO2, DCM to DCM/MeOH 9:1)