反应详情

温度

95 °C

0.140 g (261 μmol) of diethyl 2-(4-tert-butoxycarbonylaminobutyl)-2-[1-(5-cyclopropyl-[1,3,4]thiadiazol-2-ylmethyl)-1H-imidazol-4-yl]malonate was suspended in 10 ml of semi-concentrated hydrochloric acid, and the mixture was heated with stirring at 95° C. for 8 h. The reaction mixture was concentrated under reduced pressure and purified by preparative HPLC, and the product-containing fractions were freeze-dried and then taken up in 2.5 eq of 1N hydrochloric acid and freeze-dried and taken up in water and freeze-dried. The preparation was then purified once more by preparative HPLC, and the product-containing fractions were freeze-dried. This gave 35 mg (32%) of the title compound as trifluoroacetic acid salt.

1. temperaturethe mixture was heated
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. custompurified by preparative HPLC
4. customthe product-containing fractions were freeze-dried
5. customfreeze-dried
6. customfreeze-dried
7. customThe preparation was then purified once more by preparative HPLC
8. customthe product-containing fractions were freeze-dried