HRID602669
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
The reaction mixture of 51 mg (0.114 mmol) of 2-{1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}-2-(3,5-difluorophenyl)ethanol, 24 mg (0.137 mmol) of methanesulfonic anhydride, 14 mg (0.285 mmol) of sodium cyanide and 11 uL (0.137 mmol) pyridine in 5 mL of acetonitrile was stirred for 12 h at rt, and then concentrated. The residue was purified by silica gel chromatography with hexanes/ethyl acetate to the title compound; 1NMR (CDCl3) δ 3.29 (s, 2H), 3.96 (s, 2H), 4.01 (s, 2), 4.54 (s, 1H), 6.69-6.75 (m, 3H), 7.29-6-7.7.38 (m, 8H); Mass Spectrum m/e=455 (M+1 35Cl, 35Cl) and 457 (M+1 35Cl, 37Cl).
WORKUP
后处理
- concentrationconcentrated
- customThe residue was purified by silica gel chromatography with hexanes/ethyl acetate to the title compound