反应详情

Propargyl alcohol (50 mg), cuprous iodide (50 mg) and a solution of PdCl2(PPh3)2 (1 mL, 0.15 M in THF) are added to a suspension of N-(4-chlorobenzyl)-9-iodo-1-methyl-2,7-dioxo-2,3-dihydro-1H,7H-pyrido[1,2,3-de]quinoxaline-6-carboxamide (Preparation 23, 250 mg) in diethylamine (2.0 mL). The reaction is stirred for 90 min and the product is then extracted into chloroform and is chromatographed on silica gel. The desired product is eluted with 20% methanol/chloroform. Physical characteristics: 1H NMR (DMSO-d6) δ3.40, 4.36, 4.56, 5.22, 5.42, 7.36, 7.40, 7.44, 7.88, 8.76, 10.2. HRMS m/z 436.1064 (C23H18ClN3O4).

1. extractionthe product is then extracted into chloroform
2. customis chromatographed on silica gel
3. washThe desired product is eluted with 20% methanol/chloroform