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温度

0 °C

A solution of chlorosulfanic acid (3 mL) is cooled to 0° C. and 1-ethyl-3-phenylthiourea (360 mg, 2.0 mmol) is then added over a period of 5 minutes and the resulting mixture is stirred at 0° C. for 2 hour followed by addition of water (10 mL) which results in the formation of a precipitate. EtOAc is added to dissolve the precipitate and the mixture is extracted (5×15 mL). The combined organic layers are concentrated and dissolved in a mixture of dioxane and water (12 mL, 1:1). The resulted mixture is heated to 80° C. for 2 hr. and concentrated to provide 4-(3-ethylthioureido)benzenesulfonic acid (1-4) as an off white solid. HPLC-MS calculated for C9H12N2O3S2 (M+H+) 261.0. found 261.0.

1. customresults in the formation of a precipitate
2. dissolutionto dissolve the precipitate
3. extractionthe mixture is extracted (5×15 mL)
4. concentrationThe combined organic layers are concentrated
5. dissolutiondissolved in a mixture of dioxane and water (12 mL, 1:1)
6. temperatureThe resulted mixture is heated to 80° C. for 2 hr
7. concentrationand concentrated