反应详情

At room temperature, 0.12 ml (0.76 mmol) of diethyl azodicarboxylate (DEAD) is added dropwise to a suspension of 150 mg (0.49 mmol) of 5-chloro-N-(1,3-dioxo-2,3-dihydro-1H-isoindol-4-yl)-2-thiophenecarboxamide, 148 mg (0.73 mmol) of tert-butyl 4-hydroxytetrahydro-1(2H)-pyridinecarboxylate and 199 mg (0.76 mmol) of triphenylphosphine in 1.95 ml of absolute THF. After 2 h at room temperature, the mixture is concentrated and the residue is separated by chromatography on silica gel (dichloromethane/methanol mixture) and the product is isolated. Yield: 184 mg (76.8% of theory); MS (LC-MS): m/z (%)=279 (M+H, 100); LC-MS (Method 4): rt (%)=3.88 (98.9).

1. concentrationthe mixture is concentrated
2. customthe residue is separated by chromatography on silica gel (dichloromethane/methanol mixture)
3. customthe product is isolated