Reference of 460-37-7, 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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
Under nitrogen protection,Magnesium 13.4g (0.55mol) and magnesium were placed in the reaction flask.3-iodo-1,1,1-trifluoropropane7g is dissolved in 90g of tetrahydrofuran,Slowly raise the temperature to 35-40 C,After the reaction was initiated, 3-iodo-1,1,1-trifluoropropane 105g andA 220 g mixture of tetrahydrofuran was slowly added dropwise to the reaction flask to maintain the temperature at 60-65 C.After the completion of the dropwise addition, the reaction was kept for 2 hours, allowed to stand and cooled to room temperature, and the concentration was measured to be 1.64 mol/L, and the yield was 95%.Under nitrogen protection,2,5 g (0.39 mol) of N,N-dimethylformamide was placed in the reaction flask.2-methyltetrahydrofuran 70g,Cool down to -25 C to -20 C,1.64 mol/L of 1,1,1-trifluoropropyl magnesium iodide was added dropwise in this temperature range.183mL of 2-methyltetrahydrofuran solution, drip, heat for 1 hour, slowly rise to room temperature, add a small amount of water to quench and dissociate, then add 4NHydrochloric acid is adjusted to pH=3-4, and the layer is allowed to stand. The aqueous layer is extracted with a small amount of 2-methyltetrahydrofuran, and the organic phase is enriched and added.And sodium bisulfite was raised to 30-35 C for 1 hour, a large amount of solids were precipitated after cooling, filtered, and the filter cake was rinsed and dried to obtain a solid.The 4,4,4-trifluorobutanal obtained by dissociating the layer and the diluted hydrochloric acid at 35-40 C was dried over anhydrous sodium sulfate to obtain 29.5 g.Yield 78%, GC: 98.6%.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; Pulasi Science And Technology (Shanghai) Co., Ltd.; Cai Weibing; Xu Gengdu; (8 pag.)CN109369354; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com