反应详情

温度

0 °C

To a solution of 5-aminomethyl-[2-(4-cyclopropylpiperazin-1-yl)benzooxazole (500 mg, 1.84 mmol) in CH2Cl2 (15 mL) was added Et3N (929 mg, 9.2 mmol). The mixture was stirred at 0° C. for 5 min and then 3-chloropropane-1-sulfonyl chloride (326 mg, 1.84 mmol) was added dropwise. The mixture was stirred at 0° C. for 1 h and brought gradually to rt. Then the mixture was stirred for another 1 h. The volatiles were removed and the residue was extracted with CH2Cl2. The resulting residue was purified by column chromatography on silica gel (elute: 5% CH2Cl2 in methanol) to give 3-chloropropane-1-sulfonic acid [2-(4-cyclopropylpiperazin-1-yl)benzooxazol-5-ylmethyl]amide (315 mg, 42%).

1. stirringThe mixture was stirred at 0° C. for 1 h
2. custombrought gradually to rt
3. stirringThen the mixture was stirred for another 1 h
4. customThe volatiles were removed
5. extractionthe residue was extracted with CH2Cl2
6. customThe resulting residue was purified by column chromatography on silica gel (elute: 5% CH2Cl2 in methanol)