反应详情

To a solution of 4-bromo-N-(2-methylbut-3-yn-2-yl)benzenamine (3.30 g, 14 mmol) in toluene (14 ml, 14 mmol) was added copper(I) chloride (0.300 g, 3.0 mmol) in one portion. The reaction vessel was sealed and the resulting mixture was heated to 90 deg C. After stirring overnight, the mixture was transferred to a separatory funnel containing water and EtOAc. The aqueous layer was washed 1× with EtOAc and 3× with DCM. The organic layers were combined, dried with MgSO4, filtered and concentrated. The crude oil was purified with an MPLC (100% DCM to 10% (91/10/1 DCM:MeOH:NH4OH)) to provide the product. MS m/z: 238.

1. customThe reaction vessel was sealed
2. temperaturethe resulting mixture was heated to 90 deg C
3. customthe mixture was transferred to a separatory funnel
4. washThe aqueous layer was washed 1× with EtOAc and 3× with DCM
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude oil was purified with an MPLC (100% DCM to 10% (91/10/1 DCM:MeOH:NH4OH))
9. customto provide the product