反应详情

To a solution of the product of Example 4 Step A, (4.44 g, 22.1 mmol) in CH2Cl2 was added N,N-diisopropylethyl amine (1.2 eq.) and 4-dimethylaminopyridine (0.1 eq.), and t-butyldimethylsilyl chloride (1.2 eq.). The mixture was stirred for 1.5 hours at room temperature, then concentrated in vacuo. The residue was dissolved in ethyl acetate and washed with water, brine, dried (MgSO4), filtered, and concentrated in vacuo. The residue was chromatographed on silica (ethyl acetate/hexanes (2.5/97.5)) to afford 5.0 g (71%) of the title compound.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with water, brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed on silica (ethyl acetate/hexanes (2.5/97.5))