反应详情

A N2 covered solution of 1.19 g (6.6 mmol) of the product from Step 1 in 24 ml of DMF was treated with 2.07 g (32.9 mmol) of ammonium formate followed by 0.36 g of palladium on carbon catalyst. After stirring vigorously at room temperature for 17 hours, the reaction was diluted with MeOH and the catalyst was removed by filtration through celite. The filtrate was concentrated in vacuo and the residue was chromatographed over silica gel (3% MeOH: 0.3% NH4OH: CH2Cl2) to yield 0.876 g, m.p. 152°-153.5° C. (88.2%) of the titled product.

1. customthe catalyst was removed by filtration through celite
2. concentrationThe filtrate was concentrated in vacuo
3. customthe residue was chromatographed over silica gel (3% MeOH: 0.3% NH4OH: CH2Cl2)