460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 460-37-7
1,2-Dibromoethane (0.04 ml, 0.51 mmol) was added to a stirred suspension of zinc (0.45 g, 6.82 mmol) in DMF (3.5 ml). The mixture was stirred at 90 C for 30 min. under nitrogen and then chlorotrimethylsilane (0.013 ml, 0.102 mmol) was added. The mixture was stirred at RT for a further 30 min. and then a solution of 3-iodo-l,l,l- trifluoropropane in DMF (2 ml) was added dropwise . The mixture was stirred at 45 C for 2.5 h. and the resulting solution was transferred via syringe to a second flask charged with intermediate 34 (0.144 g, 0.34 mmol) andbis(triphenylphosphine)palladium (II) dichloride (0.024 g, 0.034 mmol) under nitrogen. The mixture was stirred at 40 C for 1 h. and then allowed to cool down to RT. A saturated solution of ammonium chloride was added and the mixture was extracted with EtOAc. The organic layer was separated, washed with a saturated solution of ammonium chloride and brine, dried (Na2S04), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; EtOAc in heptane 0/100 to 100/0). The desired fractions were collected and evaporated in vacuo to yield intermediate 38 (0.07 g, 52%) as a pale brown solid.
The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose, Manuel; CONDE-CEIDE, Susana; MACDONALD, Gregor, James; PASTOR-FERNANDEZ, Joaquin; VAN GOOL, Michiel, Luc, Maria; MARTIN-MARTIN, Maria, Luz; VANHOOF, Greta, Constantia, Peter; WO2011/110545; (2011); A1;,
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