Introduction of a new synthetic route about 1017779-69-9

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Fluoro-4-(trifluoromethoxy)aniline, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1017779-69-9, name is 3-Fluoro-4-(trifluoromethoxy)aniline, belongs to ethers-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 1017779-69-9, HPLC of Formula: C7H5F4NO

[0193j Step 1[0194j Corresponding amine (1 equiv.) and triethylamine (1.5 equiv.) was dissolved in CH2C12 (54 mM corresponding to amine) and stirred at -78 C. Triphosgene (0.45 equiv.) dissolved in CH2C12 (20 mM, corresponding triphosgene) was added dropwise at -78 C. The reaction was then warm to rt and was stirred for 30 mm. The reaction was cooled to 0 C. Corresponding piperidine (1.5 equiv.) and triethylamine (1.5 equiv.) dissolved in CH2C12 (54 mM, corresponding piperidine) was added slowly and the reaction was further stirred at rt for 12 h. The reaction was quenched with the addition of HC1 solution (2M). The organic layer was collected and the aqueous layer was further extracted with EtOAc (EtOAc: Aqueous layer 1:1) for three times. The combined organic layer was washed with sat. NaC1 solution. The organic layer was dried over anhydrous magnesium sulfate and was concentrated in vacuo. The product was used without further purification.[0277j The reaction was carried out according to synthetic pathway 2. The 3-fluoro-4- (trifluoromethoxy)aniline (109 mg, 559 jimol) was reacted with 1-(4-aminopiperidin-1-yl)-2- methylpropan-1-one (143 mg, 838 jimol). The product was purified by flash chromatography using ethyl acetate :hexane (7:3). The product was further purified by recrystallization using methanol and water.[0278j Yield: 150 mg, 383 jimol, 68.6% yield. Purity (H-NMR): 95%

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Fluoro-4-(trifluoromethoxy)aniline, and friends who are interested can also refer to it.

Reference:
Patent; EICOSIS, LLC; HAMMOCK, Bruce, D.; LEE, Kin, Sing, Stephen; INCEOGLU, Ahmet, Bora; WO2015/148954; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem