Application of 3597-91-9, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 3597-91-9 as follows.
Step 1. Preparation of biphenyl-4-ylmethy. 2,2,2-trichloroethanimidoate (C93). A suspension of biphenyl-4-yimethanol (36.8 g, 200 mmol) in dichloromethane (240 mL) was treated with 50% aqueous potassium hydroxide solution (160 mL). The reaction mixture was cooled to 0″C, and maintained at 0 – 1OC as tetra-rt-butylammonium sulfate (1.18 g, 2,0 mmol) was added, followed by a slow addition of trichtoroacetonitrile (25.1 mL, 250 mmol) over 10 minutes. The reaction was stirred at OC for an hour, and then stirred at 25C for an additional hour, after which the organic layer was filtered through a short pad of Celite on top of a layer of silica gel. The pad was rinsed with additional methylene chloride (1500 mL), and the elubetants were concentrated in vacuo to provide C93 as a white solid, which was used in the next step without purification. Yield: 66.1 g, quantitative. LCMS m/z 167.2 (C13H1 1′). 1H NMR (400 MHz, CDCI3) 6 5.40 (s, 2H), 7,37 (m, 1 H), 7.46 (m, 2H), 7.52 (d, J?8.7 Hz, 2H), 7,62 (m, 4H), 8.43 (br s, 1 H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3597-91-9, its application will become more common.
Reference:
Patent; PFIZER INC.; BROWN, Matthew Frank; DONOVAN, Charles Francis; ELLSWORTH, Edmund Lee; HOYER, Denton Wade; JOHNSON, Timothy Allen; LALL, Manjinder Singh; LIMBERAKIS, Chris; MURPHY, Sean Timothy; SHERRY, Debra Ann; TAYLOR, Clarke Bentley; WARMUS, Joseph Scott; WO2010/32147; (2010); A2;,
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