反应详情

A solution of 6-(2-furyl)-1H-purine-2-amine (25 mg, 0.12 mmol) in anhydrous DMF (0.5 mL) and anhydrous THF (2 mL) was treated with triphenylphosphine polystyrene (65 mg, 0.25 mmol) and 2-cyclohexylethanol (35 mg, 0.25 mmol), shaken at room temperature for 10 min, treated with di-tert-butyl azodicarboxylate (0.058 g, 0.25 mmol), shaken at room temperature for 16 h, filtered and concentrated in vacuo. The resulting oil was dissolved in CH2Cl2 (2 mL) and TFA (1 mL), shaken for 2 h and concentrated in vacuo. The resulting oil was dissolved in CH2Cl2 (3 mL), shaken with 1-M aq HCl (1 mL) for 15 min and the organic phase concentrated in vacuo and purified by chromatography (SiO2; EtOAc) to give the title compound (22 mg, 57%) as a yellow solid.

1. stirringshaken at room temperature for 16 h
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. dissolutionThe resulting oil was dissolved in CH2Cl2 (2 mL)
5. stirringTFA (1 mL), shaken for 2 h
6. concentrationconcentrated in vacuo
7. dissolutionThe resulting oil was dissolved in CH2Cl2 (3 mL)
8. stirringshaken with 1-M aq HCl (1 mL) for 15 min
9. concentrationthe organic phase concentrated in vacuo
10. custompurified by chromatography (SiO2; EtOAc)