627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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. Computed Properties of C3H6I2
Example 39 l-(2-[(2,6-difluorophenyl)methoxyl-l,l,l,3,3,3-hexafluoropropan-2-yl|-4-[l-(4- fluorobenzenesulfonyl)cyclobutyl”|benzene Sodium hydride (14.75 mg, 0.369 mmol, 60%> suspension in mineral oil) was added to a solution of l,3-difluoro-2-(((l,l,l,3,3,3-hexafluoro-2-(4-(((4- fluorophenyl)sulfonyl)methyl)phenyl)propan-2-yl)oxy)methyl)benzene (20 mg, 0.037 mmol) and 1,3-diiodopropane (10.91 mg, 0.037 mmol) in Nu,Nu-dimethylformamide (1 mL). After 1 h at room temperature, saturated ammonium chloride (2 mL) and ethyl acetate (15 mL) were added. The mixture was washed with water (2×5 mL), brine (5 mL), dried (magnesium sulfate), filtered and concentrated under reduced pressure. The crude material was purified via preparative LC/MS with the following conditions: Column: Waters XBridge CI 8, 19 x 150 mm, 5-muiotaeta particles; Mobile Phase A: 5:95 acetonitrile: water with 10-mM ammonium acetate; Mobile Phase B: 95:5 acetonitrile: water with 10-mM ammonium acetate; Gradient: 40-100% B over 15 minutes, then a 5-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation to give Example 39 (13.2 mg, 62% yield). LC/MS (M+18): 600.1; LC retention time: 2.296 (analytical HPLC Method B); 1H NMR (500 MHz, 1 : 1 mixture of CDCI3-CD3OD) delta ppm 7.56 (d, J=8.4 Hz, 2H), 7.50 – 7.41 (m, 1H), 7.38 – 7.30 (m, 2H), 7.19 (d, J=8.4 Hz, 2H), 7.11 – 6.97 (m, 4H), 4.70 (s, 2H), 3.27 (ddd, J=13.9, 9.9, 5.9 Hz, 2H), 2.81 – 2.67 (m, 2H), 2.45 – 2.30 (m, 1H), 2.13 – 1.97 (m, 1H).
The synthetic route of 627-31-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; DUAN, Jingwu; DHAR, T. G. Murali; JIANG, Bin; LU, Zhonghui; KARMAKAR, Ananta; GUPTA, Arun Kumar; WEIGELT, Carolyn A.; WO2015/103508; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com