Reference of 770-71-8, 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 770-71-8 as follows.
Example 1 Synthesis of (chloromethyl) (1-adamantylmethyl) ether represented by a structural formula: A Kjeldahl flask having a volume of 50 ml equipped with a nozzle for introducing hydrogen chloride gas was charged with 1.66 g (10 mmol) of 1-adamantylmethanol, 0.60 g (20 mmol) of paraformaldehyde, 1.20 g (10 mmol) of magnesium sulfate and 30 ml of dried dichloromethane, and it was cooled to 0C on an ice bath and stirred. Hydrogen chloride gas generated by mixing 10 g of sodium chloride with 50 ml of conc. sulfuric acid was blown thereinto through the nozzle for one hour. After further stirring for 60 minutes, magnesium sulfate was filtered, and then the solution was analyzed by gas chromatography to confirm that 1-adamantylmethanol was completely converted and that the intended product was obtained at a selectivity of 94.5 %. Hydrogen chloride and dichloromethane were removed, and then refining was carried out by distillation to isolate 1.87 g (8.72 mmol, yield 87.2 %) of the intended product. The analytical results of the above compound are shown below. ¡¤Nuclear magnetic resonance spectrometry (NMR): CDCl31H-NMR (500 MHz): 1.53 (6H, f), 1.64 to 1.72 (6H, d), 1.97 (3H, e), 3.25 (2H, b), 5.50 (2H, a),13C-NMR (126 MHz): 28.18 (e), 37.11 (d or f), 39.45 (d or f), 33.49 (c), 81.34 (b), 84.25 (a) ¡¤Infrared spectrometry (IR): 2905 cm-1 (C-H; str.), 1157 cm-1 (C-O-C; str.), 650 cm-1 (C-Cl; str.) ¡¤ Boiling point (bp): 130 to 133C/0.7 kPa
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,770-71-8, its application will become more common.
Reference:
Patent; IDEMITSU KOSAN COMPANY LIMITED; EP1577285; (2005); A1;,
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