反应详情

To a solution of compound 6 (0.36 g, 1.1 mmol) in 1,2-dichloroethane (10 mL) containing proton sponge (0.02 g), cooled in an ice-water bath under an argon atmosphere, was added dropwise 1-chloroethyl chloroformate (0.3 mL, 3.1 mmol). The resultant solution was boiled at reflux for 4 hours, cooled and was concentrated in vacuo. The residue obtained was mixed with methanol (10 mL) and heated under reflux for 2 hours, then cooled and concentrated in vacuo to give the hydrochloride salt of 3-(4-chlorophenyl)azetidine (7) which was used without further purification.

1. temperaturecooled in an ice-water bath under an argon atmosphere
2. temperatureat reflux for 4 hours
3. temperaturecooled
4. concentrationwas concentrated in vacuo
5. customThe residue obtained
6. temperatureheated
7. temperatureunder reflux for 2 hours
8. temperaturecooled
9. concentrationconcentrated in vacuo