反应详情

温度

120 °C

The methyl ester from Step I (285 mg, 0.54 mmol) was dissolved in a 4:2:1 mixture of THF:H2O:methanol (7 mL), LiOH.H2O (225 mg, 5.36 mmol) was added to solution, and it was heated in a microwave oven at 120° C. for 5 min, then for an additional 5 min at 130° C. The reaction mixture was diluted with CH2Cl2, acidified with 2N HCl, washed with brine, and organic fraction was dried over Na2SO4 and evaporated to dryness. The residue was purified by column chromatography on silicagel eluting with 0-10% MeOH in CH2Cl2 to give 265 mg (95%) of 5-(4,4-dimethyl-cyclohex-1-enyl)-3-[(trans-4-methoxymethoxy-cyclohexyl)-(trans-4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid.

1. washwashed with brine, and organic fraction
2. dry with materialwas dried over Na2SO4
3. customevaporated to dryness
4. customThe residue was purified by column chromatography on silicagel
5. washeluting with 0-10% MeOH in CH2Cl2