1,2-Dichloroethane → HCID 131720862、化合物

関与物質

反応手順

To a solution of N,N-dimethyl-2-methylpropionamide (615 mg) in 1,2-dichloroethane (20 mL) at 0° C. was added triflic anhydride (1.51 g) dropwise followed by a solution of 2,4,6-collidine (715 mg) and (E)-1-(methylthio)-4-(2-phenylethenyl)benzene (730 mg, method 1) in 1,2-dichloroethane (5 mL). The mixture was stirred at r.t. for 30 min., heated at reflux for 6 hr, cooled to r.t., and the solvent evaporated. The residue was dissolved in CCl4 (50 mL) and H2O (50 mL) and the mixture refluxed for 18 hr. The organic phase was separated, the aqueous phase extracted with CH2Cl2 (2×), the combined organic phase were dried (MgSO4) and the solvents evaporated. The resulting residue was purified by flash chromatography (silica gel; toluene) to provide title product.

情報源と証拠