反应详情

The process is performed according to the method described in Example 10 (step 10.5.). Starting with 1.00 g (2.81 mmol) of ethyl [2-(5′-bromo-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl)ethyl]carbamate, prepared in the preceding step, 0.61 g (3.37 mmol) of pinacol 2-methyl-1-propenylboronate (commercial), 2.74 g (8.42 mmol) of caesium carbonate, suspended in 18 mL of a 9/1 mixture of tetrahydrofuran and water, and 0.23 g (0.28 mmol) of PdCl2dppf.CH2Cl2, and after purifying on a column of silica gel, eluting with a 99/1/0.1 mixture of dichloromethane, methanol and 28% aqueous ammonia, 0.75 g of expected product is obtained in the form of a wax.

1. customCH2Cl2, and after purifying on a column of silica gel
2. washeluting with a 99/1/0.1 mixture of dichloromethane, methanol and 28% aqueous ammonia