反应详情

A mixture of 3-[2-(trifluoromethyl)-2′-fluoro-4′-bromobenzhydryloxy]-N-(tert-butyl)-azetidine-1-carboxamide (115) (106 mg, 0.21 mmol), diglyme (1 mL), 4M K2CO3 (0.2 mL), toluene (1 mL), (R/S)-BINAP (12.1 mg), Herrmann's catalyst [CAS: 172418-32-5] (7.0 mg), Mo(CO)6 (26.0 mg) and piperidine (27 μL) was irradiated, with stirring, in a microwave reactor. Power was applied and varied to maintain the reaction at a temperature of 150° C. for a period of 15 min. After this time, the reaction was allowed to cool, then was filtered and evaporated. Purification by flash column chromatography [SiO2; ethyl acetate-iso-hexane (30:70→70:30)] afforded 3-[2-(trifluoromethyl)-2′-fluoro-4′-(1-piperidinyloxomethyl)benzhydryloxy]-N-(tert-butyl)azetidine-1-carboxamide (184) as a pale yellow solid (13.2 mg, 12%)

1. customwas irradiated
2. temperatureto maintain
3. customthe reaction at a temperature of 150° C. for a period of 15 min
4. temperatureto cool
5. filtrationwas filtered
6. customevaporated
7. customPurification by flash column chromatography [SiO2; ethyl acetate-iso-hexane (30:70→70:30)]