311-86-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 311-86-4, name is 2-Bromo-3,3,3-trifluoropropan-1-ol, molecular formula is C3H4BrF3O, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
To a cold mixture of triphosgene (0.9 equiv.) and 2-bromo-3,3,3-trifluoropropan-1-ol (2equiv.) in THF was added pyridine (2 equiv.). The mixture was stirred at 0 C for 30 mm. In a separate flask, a suspension of Intermediate 2 (1 equiv.) in pyridine (2 equiv.) was cooled to 0C. To this suspension was added the mixture of triphosgene and bromopropanol via syringe, and the resulting mixture was heated to 60 C for 24 h. Contents were concentrated in vacuo, and the residue was diluted with ethyl acetate and washed with iN HC1 solution. The organic layer was dried over Mg504, filtered, and concentrated in vacuo to give a crude oil. The oil was purified via silica gel chromatography utilizing a 0-100% ethyl acetate/hexanes gradient todeliver the desired carbamate intermediate, 2-bromo-3,3,3-trifluoropropyl(2-( 1 -(2-fluorobenzyl)-5 -(isoxazol-3 -yl)- 1 H-pyrazol-3 -yl)pyrimidin-4-yl) carbamate (77 mg, 4% yield) as a light brown oil.1H NMR (500 MHz, CDC13) oe ppm 8.46 – 8.48 (m, 1 H), 8.07 (br. s., 1 H), 7.86 (d, 1 H), 7.44 -7.47 (m, 1 H), 7.17 – 7.24 (m, 1 H), 7.00 – 7.07 (m, 1 H), 6.93 – 7.00 (m, 1 H), 6.78 – 6.85 (m, 1 H), 6.57 – 6.62 (m, 1 H), 6.02 (s, 2 H), 4.28 (quind, 1 H), 3.93 – 4.15 (m, 2 H).
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. 311-86-4, 2-Bromo-3,3,3-trifluoropropan-1-ol, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; NAKAI, Takashi; MOORE, Joel; PERL, Nicholas Robert; IYENGAR, Rajesh R.; MERMERIAN, Ara; IM, G-Yoon Jamie; LEE, Thomas Wai-Ho; HUDSON, Colleen; RENNIE, Glen Robert; JIA, James; RENHOWE, Paul Allen; BARDEN, Timothy Claude; YU, Xiang Y; SHEPPECK, James Edward; IYER, Karthik; JUNG, Joon; WO2014/144100; (2014); A2;,
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