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 20691-72-9 as follows. 20691-72-9
Method c: To a solution of the 4-iodo-2-nitroaniline (550 mmol) and DMAP (1.22 g, 10 mmol) in THF (1000 mL) at 23 C. was dropwise added within 70 min a solution of Boc2O (246 g, 1128 mmol) in THF (500 mL) and stirring was continued at 23 C. for 75 min. The entire mixture was evaporated to dryness and dried at HV to leave a dark brown solid (253.59 g). This material was dissolved in DCM (1100 mL), cooled to 0 C. and TFA (84 mL, 1100 mmol) was added dropwise. The mixture was stirred at 0 C. for 2 h, poured into icecold sat. NaHCO3-sol., extracted with DCM, washed with brine and dried over MgSO4. Removal of the solvent in vacuum left a dark brown solid (199.71 g) which was coated on silica gel and purified by silica gel column chromatography with hexane/EtOAc to give the (4-iodo-2-nitro-phenyl)-carbamic acid tert.-butyl ester as a yellow solid.
According to the analysis of related databases, 20691-72-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Hoffmann-la Roche Inc.; US6407094; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com