反应详情

温度

70 °C

A mixture of 3-[(5-chloro-1,3-benzothiazol-2-yl)methoxy]-2,6-difluorobenzene-carbonitrile (250 mg, 0.74 mmol, 1 equiv.), Na2CO3 (181 mg, 1.70 mmol, 2.3 equiv.) and hydroxylamine hydrochloride (103 mg, 1.48 mmol, 2 equiv.) in absolute EtOH (5 ml) was stirred at 70° C. for 8 h. Excess Na2CO3 (181 mg, 1.70 mmol, 2.3 equiv.) and hydroxylamine hydrochloride (103 mg, 1.48 mmol, 2 equiv.) were added and the heating continued for 1 h. The reaction mixture cooled at room temperature, diluted with water (40 ml) and extracted with CH2Cl2 (3×60 ml). The combined organic extracts were dried (MgSO4) and evaporated to dryness under reduced pressure, to give 201 mg (73% yield) of the desired product. Mp 169-170° C., HPLC (Gemini C18, 50×4.6 mm): m/z 370 [M+H]+, Rt=3.82 min.

1. waitthe heating continued for 1 h
2. temperatureThe reaction mixture cooled at room temperature
3. extractionextracted with CH2Cl2 (3×60 ml)
4. dry with materialThe combined organic extracts were dried (MgSO4)
5. customevaporated to dryness under reduced pressure