反应详情

温度

85 °C

The mixture of 4-(2-((S)-1-(2-fluorophenyl)ethylamino)-5-methyl-4-oxo-4,5-dihydrothiazol-5-yl)benzonitrile (0.080 g, 0.23 mmol) and potassium hydroxide (VWR, 0.17 g, 2.9 mmol) and t-BuOH (2 mL) was gradually heated to 85° C. The solid gradually dissolved and the mixture became a solution. After 1 h, the reaction was added to 2N HCl until the pH was ca. 7-8. The mixture was extracted three times with CH2Cl2, and the combined organic layers was dried over Na2SO4, filtered, and concentrated in vacuo. The crude was purified by silica gel chromatography. MS: 372 (M+1), 370 (M−1).

1. dissolutionThe solid gradually dissolved
2. extractionThe mixture was extracted three times with CH2Cl2
3. dry with materialthe combined organic layers was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude was purified by silica gel chromatography