反应详情

温度

65 °C

120 mg of powdered NaOH and 141 mg of N-methyltrichloro-acetamide (0.8 mmol) were added to 299 mg (0.8 mmol) of 2-[2-(5-chloro-2-methoxybenzoylamino)ethyl]-5-sulfamoyl-thiophene in 9 ml of DMSO. The mixture was stir 65° C. for 1.5 hours. After cooling, it was stirred into ice water of pH 2. The precipitate was filtered off with suction and taken up in CH2Cl2, and the solution was washed with water and dried using MgSO4. After evaporating the solvent, a yellow-brown crude product remained which, after treatment with CH2Cl2 /5% methanol, crystallized at -4° C.

1. temperatureAfter cooling
2. filtrationThe precipitate was filtered off with suction
3. washthe solution was washed with water
4. customdried
5. customAfter evaporating the solvent
6. customafter treatment with CH2Cl2 /5% methanol, crystallized at -4° C.