反应详情

To a solution of 3-chloropropane-1-sulfonyl chloride (1.46 g, 8.22 mmol) in anhydrous CH2Cl2 (20 mL) at 0° C. is added bis-(4-methoxy-benzyl)-amine (2.22 g, 8.63 mmol) followed by Et3N (1.68 g, 10.69 mmol). After the addition, the mixture is allowed to warm to room temperature and is stirred for 2 h. The mixture is then poured into water (50 mL) and is extracted with CH2Cl2 (3×50 mL). The combined organic layers are concentrated and purified by flash column chromatography (silica gel, EtOAc/hexane 0%˜50%) to provide 3-chloro-N,N-bis(4-methoxybenzyl)propane-1-sulfonamide as colorless oil. (2.7 g, 84%).

1. additionAfter the addition
2. extractionis extracted with CH2Cl2 (3×50 mL)
3. concentrationThe combined organic layers are concentrated
4. custompurified by flash column chromatography (silica gel, EtOAc/hexane 0%˜50%)