反应详情

Gently stir for 30 min a mixture of polymer supported triphenylphosphine (1.0 g, 3 mmol/g, 3.0 mmol), 1H-imidazole (208 mg, 3.06 mmol), and iodine (776 mg; 3.06 mmol) in anhydrous dichloromethane (12 mL). To the reaction mixture, add a mixture of N-(4-(hydroxymethyl)benzyl)-1-methyl-1H-imidazole-4-carboxamide (500 mg, 2.04 mmol) in anhydrous dichloromethane (5.0 mL). Gently stir the reaction mixture for 5 hrs at room temperature. Filter the reaction mixture and wash the filtrate with an aqueous 10% sodium thiosulfate solution. Separate the aqueous layer. Wash the organic layer with water, dry over magnesium sulfate, and concentrate to the title compound (532 mg, 1.50 mmol). MS (m/z): 356 (M+1).

1. additiona mixture of polymer
2. additionTo the reaction mixture, add
3. stirringGently stir the reaction mixture for 5 hrs at room temperature
4. filtrationFilter the reaction mixture
5. washwash the filtrate with an aqueous 10% sodium thiosulfate solution
6. customSeparate the aqueous layer
7. washWash the organic layer with water
8. dry with materialdry over magnesium sulfate