反应详情

A solution of 4-((5-(4-(bis(4-methoxybenzyl)amino)-6-methyl-1,3,5-triazin-2-yl)-6-(6-methoxypyridin-3-ylamino)pyridin-3-yl)(hydroxy)methyl)-N,N-dimethylbenzenesulfonamide (12.9 mg, 0.017 mmol) in DCM (0.2 mL) was treated with pyridine (20 μL, 0.25 mmol) followed by methanesulfonyl chloride (20 μL, 0.258 mmol). The mixture was allowed to stand overnight. Some crystals formed. The crystals were colorless and insoluble in DCM, but soluble in water. The mixture was diluted with DCM (10 mL) and washed with saturated aqueous NaHCO3 (5 mL). The DCM layer was dried and concentrated to give a yellow solid which was soluble in DCM, but insoluble in EtOAc and sparingly soluble in dioxane. The crude product was taken on directly to the next step.

1. customSome crystals formed
2. washwashed with saturated aqueous NaHCO3 (5 mL)
3. dry with materialThe DCM layer was dried
4. concentrationconcentrated
5. customto give a yellow solid which