反应详情

温度

70 °C

Sodium hydride (60% in mineral oil, 0.08 g, 1.9 mmol) was added to (2R,5R)-2-(hydroxy-thiazol-2-yl-methyl)-5-methyl-piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.393 g, 0.95 mmol) in THF (4.8 mL) at 0° C. (ice bath) under nitrogen. The reaction was heated to 70° C. for 18 h. The reaction was cooled to room temperature and saturated aqueous ammonium chloride was added and the mixture extracted with EtOAc (3×). The combined organic extracts were dried with sodium sulfate, filtered and concentrated. Chromatography (silica gel, gradient elution, 0-100%, EtOAc in petrol 40-60) gave the title compound (0.111 g) MS: [M+H]+=314.

1. temperatureThe reaction was cooled to room temperature
2. extractionthe mixture extracted with EtOAc (3×)
3. dry with materialThe combined organic extracts were dried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. washChromatography (silica gel, gradient elution, 0-100%, EtOAc in petrol 40-60)