反应详情

Amine 47 (200 mg) was dissolved in anhydrous DMF (5 mL). Methane-sulfonyl chloride (39 μL) and DIPEA (0.175 mL) were added and the reaction mixture was stirred at rt for 18 h before being partitioned between chloroform and 1M hydrochloric acid. The aqueous phase was extracted three more times with chloroform and the combined organic extracts were dried (MgSO4), filtered and concentrated in vacuo. Purification was achieved using flash chromatography, eluting with a gradient of 1/1 EtOAc/(50/70) petroleum ether to EtOAc to yield a light brown solid, 40 mg, 17%. Rf=0.12 (1/1 EtOAc/(50/70) petroleum ether).

1. custombefore being partitioned between chloroform and 1M hydrochloric acid
2. extractionThe aqueous phase was extracted three more times with chloroform
3. dry with materialthe combined organic extracts were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification
7. washeluting with a gradient of 1/1 EtOAc/(50/70) petroleum ether to EtOAc
8. customto yield a light brown solid, 40 mg, 17%