反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Powdered 1-chloro-isoquinoline-5-sulfonyl chloride (124 mg, 0.473 mmol) is added to a stirred solution of N1-[3-(2-benzyl-4-chloro-phenoxy)-propyl]-N1-[bis-(4-methoxy-phenyl)-methyl]-ethane-1,2-diamine (258 mg, 0.473 mmol) and NEt3 (0.198 mL, 1.42 mmol) in anhydrous CH2Cl2 (5 mL) at ambient temperature under nitrogen. The resultant mixture is allowed to stir for 1 hour. The mixture is chromatographed on silica gel (gradient 0-4% EtOAc in CH2Cl2) to give 285 mg (0.370 mmol, 78% yield) of the title compound as foam. ESIMS: m/z 768 [(M−H)−, 35C, 35Cl], 770 [(M−H)−, 35Cl, 37Cl], 772 [(M−H)−, 37Cl, 37Cl. Analysis for C42H41Cl2N3O5S: calcd: C, 65.45; H, 5.36; N, 5.45; found: C, 65.43; H, 5.27; N, 5.42.
WORKUP
后处理
- customThe mixture is chromatographed on silica gel (gradient 0-4% EtOAc in CH2Cl2)