Adding a certain compound to certain chemical reactions, such as: 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 460-37-7, Application In Synthesis of 1,1,1-Trifluoro-3-iodopropane
A THF (75 mL) suspension of Zn (from Aldrich, dust, 325 mesh, 30.0 g, 461 mmol) was stirred under N2 at ambient temperature for 10 min. Afterward, 1,2-dibromoethane (from Aldrich, 4.75 g, 25.3 mmol) was added. The resulting mixture was brought to reflux times with a heat gun under N2, and then cooled to ambient temperature in a water bath. These reflux and cooling steps were repeated two more times. The mixture was then cooled to 0C in an ice bath. Chlorotrimethylsilane (from Aldrich, 3.42 mL, 26.9 mmol) was slowly added to the cooled mixture over a period of a few minutes. The resulting mixture was stirred at 0C for 5 min, and then allowed to warm to ambient temperature over 15 min while continuing to be stirred. Afterward, the mixture was cooled to 0C, and then slowly treated with 1, 1, L-TRIFLUORO-3-IODOPROPANE causing an exothermic reaction. The mixture was warmed to ambient temperature and stirred for 1 hr. The mixture was then diluted with N, N-dimethylacetamide (10 mL) to afford an organozinc reagent. Separately, an N, N-dimethylacetamide (40 mL) solution of the product from Part E (2.0 g, 3.3 mmol) was treated with bis (benzonitrile) dichloropalladium (II) (from Aldrich, 0.08 g, 0.208 mmol) and 2- (DICYCLOHEXYLPHOSPHINO)-2′-METHYLBIPHENYL (0.127 g, 0.349 mmol) under N2. The organozinc reagent (2.2 mL of stock solution, 9.78 mmol) was then added to the mixture. The resulting mixture was stirred at 55C for 4 hr, and then allowed to cool to ambient temperature overnight. Subsequently, the reaction was quenched with saturated aqueous NAHC03 (20 mL). The mixture was then partitioned further with ethyl acetate (100 mL) and de-ionized water (50 mL). The resulting biphasic mixture was filtered through Celite (pre-washed with ethyl acetate). The filter cake, in turn, was washed with ethyl acetate. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (50 mL). The combined organic layers were washed with saturated aqueous NAHCO3 (2×25 mL), washed with 1: 1 brine/de-ionized water (2×25 mL), washed with brine (2×25 mL), dried over NA2S04, filtered, and concentrated in vacuo. The resulting solid was diluted in diethyl ether, and then concentrated in VACUO, FORMING a glassy solid. This solid was triturated with 1: 1 diethyl ETHER/HEXANES. The solids were then filtered, washed with hexanes, and dried in a vacuum oven to afford the desired ester as a brown solid (1.25 g, 76% yield). The presence of the desired ester was confirmed BY 1HU R AND L9F-NMR. LC/MS m/z = 500 [M+H], 522 [M+NA].
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; PHARMACIA CORPORATION; WO2004/48368; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com