反应详情

温度

60 °C

5-(3,3-Dimethyl-but-1-ynyl)-3-[(trans-4-hydroxy-cyclohexyl)-(trans-4-methyl-cyclohexane-carbonyl)-amino]-thiophene-2-carboxylic acid methyl ester is dissolved in a 3:2:1 mixture of THF:methanol:H2O and treated with a 1N solution of LiOH.H2O. After 2 h of stirring at 60° C., the reaction mixture is concentrated under reduced pressure on a rotary evaporator. The mixture is partitioned between ethyl acetate and water. The water layer is acidified using 0.1 N HCl. The EtOAc layer is separated and dried over Na2SO4. The solvent is removed and the residue is purified by column chromatography using methanol and dichloromethane (1:9) as eluent to obtain the title compound.

1. concentrationthe reaction mixture is concentrated under reduced pressure on a rotary evaporator
2. customThe mixture is partitioned between ethyl acetate and water
3. customThe EtOAc layer is separated
4. dry with materialdried over Na2SO4
5. customThe solvent is removed
6. customthe residue is purified by column chromatography