627-32-7,Some common heterocyclic compound, 627-32-7, name is 3-Iodo-1-propanol, molecular formula is C3H7IO, 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.
Cesium carbonate [(5.] 54 g) is added to a solution [OFN (4-CHLOROBENZYL)-4-HYDROXY 2-] (hydroxymethyl) thieno [2, [3-B]] [PYRIDINE-5-CARBOXAMIDE] (5.23 g, prepared as described in US 6,239, 142) and 2-(3-iodopropoxy)tetrahydro-2H-pyran (4.32 g, prepared by mixing equal molar amounts of 2-iodopropanol and 3, 4-dihydro-2H-pyran) in DMF (20 mL). The mixture is heated at [60 C] for 4 hours. The solvent is evaporated and the residue is dissolved in 10% [MEOH] in [CH2C12.] The mixture is washed with water and the organic layer is dried (MgSO4), filtered, and concentrated. The crude product is purified by column chromatography [(CH2CLJMETHANOL,] [95/5)] followed by recrystallization from EtOAc to afford 4.82 g of the title compound as white crystals. Physical characteristics. 1H NMR (400 [MHZ,] DMSO-d6) 8 10.55, 8.71, 7.39, 7.33, 7.29, 5.79, 4. [70,] 4.53, 4.49, 4. [38, 3.] 68,3. [37,] 2.11, 1.63, 1.53, 1.40 ; MS [(EI)] m/z 490 [(MF)] ; Anal. Found: C, 58.74 ; H, 5.66 ; N, 5.61.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Iodo-1-propanol, its application will become more common.
Reference:
Patent; PHARMACIA & UPJOHN COMPANY; FLECK, Bruce, Francis; WO2004/22567; (2004); A1;,
Iodide – Wikipedia,
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