反应详情

A stirred mixture of the crude product from Step 3, (R)-(+)-α-methylbenzylamine (1.01 ml, 0.00782 mol), N-methylmorpholine (1.69 ml, 0.0154 mol) and isopropanol (20 ml) was refluxed, under nitrogen for 5 hours and then concentrated. The residue was chromatographed on silica gel first with mixtures of MeOH--CHCl3 containing from 1-10% MeOH to give an impure product which was rechromatographed on silica gel with mixtures of EtOAc-hexane containing from 1-50% EtOAc. The product obtained in this manner was dissolved in MeOH, decolorized with activated carbon and crystallized from MeOH-EtOAc-hexane to give 0.700 g of the titled product, mp 111°-128° C. (dec.).

1. temperaturewas refluxed, under nitrogen for 5 hours
2. concentrationconcentrated
3. customThe residue was chromatographed on silica gel first with mixtures of MeOH
4. customCHCl3 containing from 1-10% MeOH to give an impure product which
5. customwas rechromatographed on silica gel with mixtures of EtOAc-hexane containing from 1-50% EtOAc
6. customThe product obtained in this manner
7. customcrystallized from MeOH-EtOAc-hexane