反应详情

A mixture of 5-chloropicolinic acid (43 mg) and N-cyclohexylcarbodiimide-N′-propyloxymethyl polystyrene resin (PS-Carbodiimide: Argonaut Technologies catalog number 80,037-1; 354 mg) in dichloroethane (4 mL) was shaken for 45 minutes. The reaction was shaken for 45 minutes more after the addition of N,N-dimethylformamide (0.1 mL). The compound prepared in Example 9 (50 mg) was added and the mixture was shaken overnight. Benzaldehyde polystyrene resin (PS-benzaldehyde: Argonaut Technologies catalog number 80,036-2; 184 mg) was then added and the reaction was shaken for 3.5 hours. Macroporous triethylammonium methylpolystyrene carbonate (MP-carbonate: Argonaut Technologies catalog number 80,026-9; 202 mg) was added and the reaction was shaken for 1.5 hours more. The mixture was then filtered and concentrated to obtain the title compound (30 mg) having the following physical data.

1. stirringThe reaction was shaken for 45 minutes
2. stirringthe mixture was shaken overnight
3. stirringthe reaction was shaken for 3.5 hours
4. stirringthe reaction was shaken for 1.5 hours more
5. filtrationThe mixture was then filtered
6. concentrationconcentrated