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0 °C

Dissolve cis-1-azido-2-methyl-cyclohexane (Preparation 31) (3.68 g, 26.41 mmol) and cyclobutanone (1.85 g, 26.41 mmol) in dichloromethane (200 mL). Cool the solution to 0° C. and add titanium chloride (15.03 g, 79.23 mmol) under nitrogen. Stir the reaction for 24 hours at room temperature. Add water (200 mL), and extract the aqueous layer with dichloromethane (3×200 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 20-50% of EtOAc/Hexane) to give 1.74 g (36%) of the title compound as a colorless oil.

1. customthe reaction for 24 hours at room temperature
2. extractionAdd water (200 mL), and extract the aqueous layer with dichloromethane (3×200 mL)
3. dry with materialCombine the organic layers and dry with Na2SO4
4. filtrationfilter
5. concentrationconcentrate
6. custompurify by flash column chromatography (silica gel, 20-50% of EtOAc/Hexane)