Electric Literature of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, its 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 a solution of 479 mg (1.68 mmol) of the compound from Ex. 34A in 20 ml of DMF were added 582 mg (4.21 mmol) of potassium carbonate, and the mixture was stirred at RT for 15 min. Then 1.17 g (5.05 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 20 h. The DMF was very substantially distilled off and the residue obtained was partitioned between semisaturated sodium chloride solution (100 ml) and ethyl acetate (50 ml). The water phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 100 g of silica gel, eluent: hexane/ethyl acetate 94:6?50:50). In this way, 517 mg (85% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.09 (s, 1H), 4.13 (d, 2H), 2.84-2.69 (m, 5H), 2.30-2.23 (m, 1H), 1.15 (d, 3H), 1.07-0.95 (m, 1H), 0.90-0.81 (m, 2H). LC/MS (Method 4, ESIpos): Rt=1.2 min, m/z=361 [M+H]+.
The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Bayer Aktiengesellschaft; Bayer Pharma Aktiengesellschaft; HAERTER, Michael; KOSEMUND, Dirk; CANCHO GRANDE, Yolanda; DELBECK, Martina; KALTHOF, Bernd; LUSTIG, Klemens; SUESSMEIER, Frank; US2020/16159; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com