反应详情

温度

85 °C

Tert-butyl 3-iodoazetidine-1-carboxylate (142 g, 0.5016 mol) and hydrazine hydrate (245.21 mL, 5.02 mol) were mixed in ethanol (284 mL) and the reaction was heated to 85° C. for 48 hours under nitrogen. The reaction was cooled and the ethanol was removed in vacuo. The residue was partitioned between water (200 mL) and dichloromethane (300 mL), the water layer was re-extracted with dichloromethane (2×200 mL), the combined organics were dried over anhydrous magnesium sulphate, filtered and concentrated in vacuo to give the title compound as a colourless oil, (88.37 g). This compound was used immediately in the next step.

1. temperatureThe reaction was cooled
2. customthe ethanol was removed in vacuo
3. customThe residue was partitioned between water (200 mL) and dichloromethane (300 mL)
4. extractionthe water layer was re-extracted with dichloromethane (2×200 mL)
5. dry with materialthe combined organics were dried over anhydrous magnesium sulphate
6. filtrationfiltered
7. concentrationconcentrated in vacuo