Synthetic Route of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
To stirred a solution of methyl-(2S)-2-(te/Y-butoxycarbonyl)-amino-2-[8-aza-bicyclo [3.2.1]-oct-3-yl]-exo-acetate (step 5 of intermediate 2, 1.0 g, 3.36 mmol) in acetonitrile (20 ml) at room temperature was added anhydrous K2CO3 (1.39g, 10.07 mmol) stirred for 10 minutes. To this reaction mixture was then added 3,3,3-trifluoropropyl iodide (0.827g, 0.43 ml, 3.69 mmol) and heated at 5O0C for 6 hours under stirring. The solvent was removed under reduced pressure and added ethyl acetate (50 ml). The organic layer was washed with water (2×20 ml), bromine (10 ml) and dried over anhydrous Na2SO4. The solvent was evaporated to yield the crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 1.3% methanol in dichloromethane as an eluent to yield the title compound (0.775g, 58%). MS: m/z 395(M+1) 1HNMR (CDCI3, 200 MHz): delta 1.17-1.60 (m, 15H), 1.82-2.40 (m, 5H), 2.5 -2.63 (m, 2H), 3.14- 3.28 (m, 2H) 3.73 (s, 3H) 4.10-4.30 (m, 1 H), 4.97-5.10 (m, 1 H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.
Reference:
Patent; LUPIN LIMITED; WO2009/37719; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com