反应详情

温度

40 °C

5-(3,3-Dimethyl-but-1-ynyl)-3-[(1,4-dioxa-spiro[4.5]dec-8-yl)-(trans-4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid methyl ester (1 eq.) is dissolved in tetrahydrofuran and treated with 3.6 N HCl solution. The reaction is stirred at 40° C. for 5 h. Water is then added and the reaction mixture is cooled to room temperature. The reaction mixture is extracted with ethyl acetate (2×50 mL). The combined extracts are washed with 25 mL of aqueous saturated NaHCO3 and 2×50 mL of water. The organic layer is concentrated to a thick oil and 50 mL of heptane is added to the mixture to precipitate the desired compound which is filtered to give of 5-(3,3-dimethyl-but-1-ynyl)-3-[(trans-4-methyl-cyclohexanecarbonyl)-(4-oxo-cyclohexyl)-amino]-thiophene-2-carboxylic acid methyl ester.

1. temperaturethe reaction mixture is cooled to room temperature
2. extractionThe reaction mixture is extracted with ethyl acetate (2×50 mL)
3. washThe combined extracts are washed with 25 mL of aqueous saturated NaHCO3 and 2×50 mL of water
4. concentrationThe organic layer is concentrated to a thick oil and 50 mL of heptane
5. additionis added to the mixture
6. customto precipitate the desired compound which
7. filtrationis filtered