反应详情

4.7 g of 3-bromophenylboronic acid, 219 mg of NiI2, 4.3 g of sodium bis(trimethylsilyl)amide, and 106 mg of trans-2-aminocyclohexanol hydrochloride were added to 14 ml of anhydrous 2-propanol and oxygen removed by passing argon through the mixture for 10 minutes. Then, a solution of 2.2 g of 3-iodo-oxetane in 1 ml of anhydrous 2-propanol was added and the mixture kept at 80° C. under microwave irradiation for 50 minutes. The mixture was then evaporated, distributed between 100 ml of water and 100 ml of EA, and the aqueous layer extracted twice using 20 ml of EA each. The organic layer was then dried using MgSO4 and evaporated. Chromatography on silica gel using EA/HEP 1:4 yielded 1.4 g of the title compound, colorless oil. Rf (EA/HEP 1:4)=0.27

1. customremoved
2. customfor 10 minutes
3. additionThen, a solution of 2.2 g of 3-iodo-oxetane in 1 ml of anhydrous 2-propanol was added
4. customthe mixture kept at 80° C. under microwave irradiation for 50 minutes
5. customThe mixture was then evaporated
6. extractionthe aqueous layer extracted twice
7. customThe organic layer was then dried
8. customevaporated