反应详情

温度

-10 °C

A suspension of 1-ethyl-3-[5-(4-methoxy-phenyl)-4-methyl-thiazol-2-yl]urea (Example 28c) (1.0 g, 3.44 mmol) in dichloromethane (15 ml) is added portionwise to chlorosulfonic acid (25 ml, excess) cooled at −10° C. The temperature is kept below 0° C. throughout the addition. The reaction mixture is left to warm up to room temperature. After 3 hours, the reaction mixture is poured carefully onto ice (2 litres). Once ice is melted, the aqueous layer is extracted with dichloromethane (DCM) (3×200 ml). The combined organic layers are washed with brine, dried over MgSO4, filtered and concentrated to afford 5-[2-(3-ethyl-ureido)-4-methyl-thiazol-5-yl]-2-methoxy benzenesulfonylchloride.

1. additionThe temperature is kept below 0° C. throughout the addition
2. waitThe reaction mixture is left
3. temperatureto warm up to room temperature
4. additionthe reaction mixture is poured carefully onto ice (2 litres)
5. extractionthe aqueous layer is extracted with dichloromethane (DCM) (3×200 ml)
6. washThe combined organic layers are washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated