In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-4-iodoaniline
[00675] Example 6: 4-[(aminocarbonyl) amino]-1-(3-chloro-4- iodophenyl)-1 H-pyrazole-3-carboxamide; [00677] Step 1: Preparation of (2E)-2- [ (3-chloro-4- iodophenyl) hydrazono] -2-cyanoacetamide; [00679] A 250 mL 2-neck flask, flushed with N2, was charged with a stir bar and 3-chloro-4-lodoaniline (19.01 g, 75 mmol) and was then cooled in acetone/ice bath to 0C. To this was added conc. HCI (19 mL) dropwise at a rate that maintained the temperature below 5C. Water (60 mL) was added followed by a solution of sodium nitrite (5.175 g, 75 mmol) in water (15 mL) over a 5 min period. After 75 mins, a solution of sodium acetate trihydrate (30.62 g, 225 mmol) in water (75 mL) was added over a 5 min. period with the temperature maintained at 5C. The resultant yellowish slurry was then used as described in the following paragraph. [00680] To a well-stirred solution of cyanoacetamide (12.61 g, 150 mmol) in water (115 mL) and ethanol (75 mL) in a 500-mL round bottom flask was added a solution of acetate trihydrate (10.5 g, 75 mmol) in water (25 mL) and this mixture was cooled to-7C in an acetone/water bath. To this solution was added the slurry from the previous paragraph dropwise over a 70-minute period with the temperature maintained at 0C ( 2C) during the addition. After 2.5 h, the cold mixture was filtered and the solids washed with water (3 X 100 mL) and air-dried. These solids were washed with methanol (4 X 100 mL) and dried in vacuo to give a yellow solid. The methanol washes were concentrated, cooled, and filtered to provide additional product.’H NMR (DMSO-d6) : 5 11.750 (m, 1 H), 7.940 (m, 1 H), 7.860 (m, 1 H), 7.822 (m, 1 H), 7.550 (m, 1 H), 7.330 (m, 1 H). MS (ESI-) for CgH6CIIN40 m/z 347.0 (M-H) -.
The synthetic route of 135050-44-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; PHARMACIA CORPORATION; WO2005/37797; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com