反应详情

温度

90 °C

300 mg (3.29 mmol) of thiosemicarbazide and 370 mg (3.27 mmol) of 2-Cyano-2-methylpropanoic acid are dissolved in dioxane (10.0 mL) and heated to 90° C. 300 μL (3.29 mmol) of POCl3 are added dropwise. The reaction is stirred at 90° C. for 1 h, cooled to RT and diluted with 1 N aq. HCl and DCM. The aq. layer is separated, 4 N aq. NaOH is added to reach pH 8 and then extracted with DCM. Then combined organic layer is washed with brine and dried. The solvent is removed under reduced pressure to afford 180 mg of 2-(5-amino[1,3,4]thiadiazol-2-yl)-2-methyl-propionitrile. Yield: 32%; ESI-MS: 169 [M+H]+; HPLC (Rt): 0.24 min (method B)

1. temperaturecooled to RT
2. customThe aq. layer is separated
3. addition4 N aq. NaOH is added
4. extractionextracted with DCM
5. washThen combined organic layer is washed with brine
6. customdried
7. customThe solvent is removed under reduced pressure