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. 654-70-6, name is 4-Cyano-3-trifluoromethylaniline belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 654-70-6
To a nitrogen flushed, 30-L kettle was charged aniline E (4.0 kg, 21.49 mol) followed by w-heptane (9 L, 2.25 vol) and H20 (10 L, 2.5 vol). The mixture was then agitated for 8 min, cooled to 5-10 C and thiophosgene (1.81 L, 2.72 kg, 23.64 mol, 1.1 equiv) was charged over 12 min, maintaining the batch temperature at 10-16 C, followed by an w-heptane (1 L, 0.25 vol) rinse. The resulting orange slurry was then warmed to 30-40 C over 1.5 h and a slight exotherm to a maximum temperature of 46.4 C was observed. After stirring for 15 h, the orange solution was sampled (>99% conversion). The batch was then heated to 36 C and the phases were allowed to separate. A rag layer was observed and most of it was purged with the bottom aqueous layer. In two portions, w-heptane (18 L, 4.5 vol) was next charged to the orange heptane layer and the solution was distilled to 1.5 vol (45-46 C, 160 mbar). The solution was diluted once more with w-heptane (8 L, 2 vol) and the batch was distilled to 1.5 vol (45-46 C, 160 mbar). The solution was then diluted with w-heptane (10 L, 2.5 vol), cooled to 30-31 C (heptane:product F, 5.3:1) and seeded with product F (10 g). Crystallization was visible within 2-3 min after seeding and the slurry was further cooled to 0-10 C over 3 h and held at 0-10 C for 2 h. The batch was then filtered, rinsed with filtrate and cold w-heptane (4 L, 1 vol) and dried at 20-25 C, under vacuum, for 13 h to yield product F (4.51 kg, 92%), with an HPLC purity of >99%, and a moisture level of 0.04%.
The synthetic route of 654-70-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MEDIVATION PROSTATE THERAPEUTICS, INC.; JAIN, Rajendra, Parasmal; ANGELAUD, Remy; THOMPSON, Andrew; LAMBERSON, Carol; GREENFIELD, Scott; WO2011/106570; (2011); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts