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. Safety of 4-Iodo-2-methylaniline
[00653] Example 4: 4-[(aminocarbonyl) amino]-1-(4-iodo-2- methylphenyl)-1 H-pyrazole-3-carboxamide; [00655] Step 1: Preparation of (2E)-2-cyano-2- [ (4-iodo-2- methylphenyl) hydrazono] acetamide; [00657] Preparation of Solution A: 2-Methyl-4-iodoaniline (23.3 g, 100 mmol) was treated with conc. HCI (25 mL) and diluted with water (100 mL). This mixture was stirred and cooled to-5 to 0C in an ice/acetone bath. To this was added a solution of sodium nitrite (6.90 g, 100 mmol) in water (20 mL) at-5 to 0C. The resultant mixture was stirred 20 min. To this was added a-5C solution of sodium acetate trihydrate (40.8 g, 300 mmol) in water (100 mL). [00658] Preparation of Solution B: Separately, cyanoacetamide (10.1 g, 120 mmol) was dissolved in water (180 mL) and ethanol (120 mL). The solution was cooled to-5C. To this was added a cooled (-5C) solution of sodium acetate trihydrate (13.6 g, 100 mmol) in water (30 mL). [00659] Solution A was added by pipette dropwise over about 30 min to Solution B at 5C to make a pasty mixture. After 3 h the mixture was filtered. The solids were then washed with ether (500 mL) and dried further to give a yellow brown solid. NMR indicated a mixture of stereomers.
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; PHARMACIA CORPORATION; WO2005/37797; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com