反应详情

In a dry flask, phenylacetyl chloride (1 equivalent) was combined with 2-trichloroacetyl pyrrole (1 equivalent) in a minimum amount of dichloromethane (DCM) to dissolve the reactants. To the resulting solution, at ambient temperature, was added aluminum trichloride (1 equivalent). After 2 hours, the reaction mixture was applied directly onto a silica gel column. Gradient elution with 10% ethyl acetate to 50% ethyl acetate in hexanes provided compound 1 in 60% yield. 1H NMR (CDCl3) δ 4.0 (s, 2H), 7.1-7.35 (m, 7H), 9.7 (br s, NH). HPLC using method B provided Rt of 4.9 minutes. LC/MS (M+1) 330.2, (M−1) 328.1.

1. dissolutionto dissolve the reactants
2. washGradient elution with 10% ethyl acetate to 50% ethyl acetate in hexanes provided compound 1 in 60% yield
3. customprovided Rt of 4.9 minutes