Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,2-Dichloro-4-iodobenzene
General procedure: A mixture of an appropriate unnatural amino acid carboxamide 6 (0.15-0.2 mmol, 1 equiv), an appropriate aryl iodide (5 equiv), Pd(OAc)2 (10 mol%) and AgOAc (2.5 equiv) in anhydrous toluene (2-3 mL) was heated at 110 C for 15-24 h under a nitrogen atm or in a sealed tube. After the reaction period, the reaction mixture was concentrated under reduced pressure to afford a crude reaction mixture, which was purified by column chromatography on neutral alumina or silica gel (eluent EtOAc:hexane) to give the corresponding arylated amino acid (see the respective Schemes/Tables for the specific entries). 3.4.27. 3-(3,4-Dichlorophenyl)-6-(1,3-dioxoisoindolin-2-yl)-N-(quinolin-8-yl)hexanamide (10c). The compound 10c was obtained after purification by column chromatography on silica gel (EtOAc:hexane 40:60) as a greencolor solid (60 mg, 75%); Rf (40% EtOAc/hexane) 0.7; mp:110e112 C; IR (DCM): 3346, 2937, 1771, 1394, 723 cm1; 1H NMR(400 MHz, CDCl3) dH 9.64 (1H, br. s), 8.78 (1H, d, J 3.2 Hz), 8.65(1H, t, J 4.5 Hz), 8.15 (1H, d, J 7.7 Hz), 7.81 (2H, dd, J1 5.2,J2 3.1 Hz), 7.70 (2H, dd, J1 5.4, J2 3.1 Hz), 7.49 (2H, d, J 4.6 Hz),7.46 (1H, dd, J1 8.3, J2 4.2 Hz), 7.39 (1H, d, J 1.4 Hz), 7.32 (1H, d,J 8.2 Hz), 7.13 (1H, dd, J1 8.2, J2 1.5 Hz), 3.67 (2H, t, J 7.3 Hz),3.36e3.29 (1H, m), 2.87 (1H, dd, J1 14.8, J2 6.4 Hz), 2.80 (1H, dd,J1 14.8, J2 8.3 Hz), 1.92e1.82 (1H, m), 1.78e1.65 (2H, m),1.60e1.52 (1H, m); 13C NMR (CDCl3, 101 MHz): dC 169.2, 168.3,148.1,143.9, 138.2, 136.3, 134.1, 133.9, 132.7, 132.0, 130.6, 130.6, 129.4,127.9, 127.3, 127.2, 123.2, 121.6, 121.6, 116.5, 45.1, 41.6, 37.7, 33.2,26.5; HRMS (ESI) calcd for C29H24Cl2N3O3 [MH] 532.1195 found532.1177.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Article; Tomar, Radha; Bhattacharya, Debabrata; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 75; 17; (2019); p. 2447 – 2465;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com