反应详情

A mixture of 7.26 g of the compound obtained in step B) and 2.08 g of the compound obtained in step A) in 150 ml of EtOH is refluxed for 1 hour 30 minutes. After cooling to RT, the mixture is concentrated under vacuum, the residue is taken up with water, rendered alkaline to pH 10 by the addition of 10% NaOH solution and extracted with DCM, the organic phase is washed with 10% NaOH solution and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. The product obtained is dissolved in acetone, a solution of 3.31 g of p-toluenesulfonic acid monohydrate in 10 ml of acetone is added dropwise and the crystalline product formed is wrung to give 6.1 g of the expected product. M.p.=164° C.

1. temperatureis refluxed for 1 hour 30 minutes
2. concentrationthe mixture is concentrated under vacuum
3. additionby the addition of 10% NaOH solution
4. extractionextracted with DCM
5. washthe organic phase is washed with 10% NaOH solution and with saturated NaCl solution
6. dry with materialdried over MgSO4
7. customthe solvent is evaporated off under vacuum
8. customThe product obtained
9. customthe crystalline product formed