Suman Thummanagoti, Chung-Ming Sun*, Chih-Hau Chen, Zhan-Hui Xu
A mixture of cyclohexanyl isocyanide (0.1g,0.92mmol,1equiv)and selenium powder (0.21g,2.76mmol,3equiv) was dissolved by dichloromethane in 5 ml CEM reactor , The vial was sealed, immediately irradiated at 90 °C (by modulation of the power) for 3~5 min. Column chromatography (hexane, Rf =0.4) ofthe crude residue yielded compound105 as a yelow oil. A mixture of N-(3-phenylpropyl) form amide (0.1 g, 0.61 mmol, 1equiv) and Cyanuric chloride (0.22g, 1.2 mmol, 2 equiv) was dissolved by dichloromethane in 5 ml CEM reactor, than triethylamine was added until to pH become 8~9 in ice bath. The vial was sealed, immediately irradiated at 90 °C (bymodulation of the power) for 5~10 min. The solution was cooled rapidly at room temperature by passing compressed air through the microwave cavity for 1 min, then diluted with CH2Cl2 and washed with a solution of buffer pH 8~10 Na2CO3. Removal of the solvent under vacuum. Ethyl formate (120 mmol) was added dropwise to phenylpropanyl amine (40 mmol) at room temperature, and the resulting mixture was refluxed for 4-6 h. The excess ethyl formate was removed under reduced pressure to yield the colorless oil.