Reference of 13194-68-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 13194-68-8 as follows.
A solution of NaNO2 (2.96 g, 42.9 mmol) in water (30 mL) was added to a mixture of 4-iodo-2- methyl-aniline (which is available from Aldrich; 5 g, 21.5 mmol) and HC1 (30 mL) at -5 C. Themixture was stilTed at -5 C for 45 mi Tin(II) chloride dihydrate (24.1 g, 107 mmol) was added and the mixture was stirred for 30 mm. The mixture was made alkaline by adding aqueous NaOH solution. The solid was filtered off and purified by chromatography (silica gel) to give (4- iodo-2-methyl-phenyl)-hydrazine (1 g, 19%). ?H NMR (300 MHz, DMSO-d6), oe ppm 7.33 (dd, J=8.5, 2.1 Hz, 1 H), 7.23 (d, J=1.3 Hz, 1 H), 6.87 (d, J=8.5 Hz, 1 H), 6.37 (s, 1 H), 3.98 (s, 2 H),2.01 (s, 3 H, overlapping with CH3 peak from residual EtOAc solvent). MS calcd. for C7H,01N2 ([M+H]j: 249, obsd. 231.8.
According to the analysis of related databases, 13194-68-8, the application of this compound in the production field has become more and more popular.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; CHUGAI SEIYAKU KABUSHIKI KAISHA; LOPEZ-TAPIA, Francisco Javier; KONG, Norman; SO, Sung-Sau; LOU, Yan; DOMINIQUE, Romyr; WO2015/86642; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com