反应详情

温度

50 °C

The product of step III was dissolved in THF (40 mL), 3N HCl (20 mL) was added to this solution, and the mixture was heated for 3 h at 50° C., then for an additional 3 h at 60° C. The mixture was brought to room temperature, extracted with CH2Cl2, washed with sodium bicarbonate and brine, organic fraction was separated, dried over Na2SO4, and concentrated under reduced pressure. Purification by column chromatography on silica gel using hexanes-EtOAc gradient to afford 726 mg (85%) of 3-[(trans-4-methoxy-cyclohexyl)-(trans-4-methyl-cyclohexanecarbonyl)-amino]-5-(4-oxocyclohexyl)-thiophene-2-carboxylic acid methyl ester.

1. customwas brought to room temperature
2. extractionextracted with CH2Cl2
3. washwashed with sodium bicarbonate and brine, organic fraction
4. customwas separated
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customPurification by column chromatography on silica gel