反应详情

To a solution of 6-hydroxyspiro[2.5]octane-5-carbonitrile (110 mg, 0.73 mmol) in DCM (3.6 mL) was added DIPEA (190 mg, 1.4 mmol) followed by the dropwise addition of methanesulfonyl chloride (92 mg, 0.80 mmol). The resulting mixture was stirred at ambient temperature for 3 hours then DBU was added and stirring continued for 16 hours. The mixture was carefully diluted with water and extracted with EtOAc (2×). The combined organic extracts were washed with 1N aqueous HCl, brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford the title compound. The residue was carried forward without further purification.

1. stirringstirring
2. waitcontinued for 16 hours
3. extractionextracted with EtOAc (2×)
4. washThe combined organic extracts were washed with 1N aqueous HCl, brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo