反应详情

t-Butyl 4-[2-(2-cyano-1-cyclopentanon-3-yl)ethyl]benzoate (0.43 g, 1.37 mmol) prepared in the Preparative Example 105 and N,N-diisopropylethylamine (0.21 g, 1.64 mmol) were dissolved in a methanol/acetonitrile (1:5) mixture, followed by the addition of 3.2 g of a 10% by weight solution of trimethylsilyldiazomethane in hexane. The obtained mixture was stirred at room temperature for 2 hours, followed by the addition of a small amount of acetic acid. The mixture this obtained was stirred and distilled to remove the solvent. The residue was dissolved in diethyl ether, washed with diluted hydrochloric acid, dilute alkali ind an aqueous solution of common salt, dehydrated and concentrated to dryness. The residue was purified by silica gel column chromatography to give the objective compound. yield: 0.23 g

1. stirringThe mixture this obtained was stirred
2. distillationdistilled
3. customto remove the solvent
4. dissolutionThe residue was dissolved in diethyl ether
5. washwashed with diluted hydrochloric acid
6. additiondilute alkali
7. concentrationconcentrated to dryness
8. customThe residue was purified by silica gel column chromatography
9. customto give the objective compound