Electric Literature of 23877-12-5, A common heterocyclic compound, 23877-12-5, name is tert-Butyl 2-bromo-2-methylpropanoate, molecular formula is C8H15BrO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE III-2 tert-Butyl 2-(4-formylphenoxy)-2-methylpropanoate 24.42 g (200 mmol) of 4-hydroxybenzaldehyde are dissolved in 250 ml of N,N-dimethylformamide and treated with 27.64 g (200 mmol) of potassium carbonate. At 100 C., 53.55 g (240 mmol) of tert-butyl alpha-bromoisobutyrate are added dropwise. The mixture is stirred for another hour, a further 200 mmol of potassium carbonate and 240 mmol of tert-butyl alpha-bromoisobutyrate are added and, after 4 hours at 100 C., 1 l of water is added. Following extraction with diethyl ether, washing with 1 N aqeuous sodium hydroxide solution and saturated sodium chloride solution and drying over magnesium sulphate, the solvent is distilled off and the residue is purified by flash chromatography on silica gel (cyclohexane?cyclohexane/ethyl acetate 20:1?10:1?5:1) and dried under reduced pressure. The target compound is obtained in the form of colourless crystals in a yield of 42%. 1H-NMR (200 MHz, CDCl3): delta=1.40 (s, 9H), 1.62 (s, 6H), 6.91 (d, 2H), 7.79 (d, 2H), 9.88 (s, 1H). MS (ESI): 265 [M+H]+.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Urbahns, Klaus; Woltering, Michael; Nikolic, Susanne; Pernerstorfer, Josef; Hinzen, Berthold; Dittrich-Wengenroth, Elke; Bischoff, Hilmar; Hirth-Dietrich, Claudia; Lustig, Klemens; US2003/32671; (2003); A1;,
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