2-Sep-21 News Share a compound : 3972-64-3

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.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C10H13Br

In a IL three-necked round-bottom flask equipped with a mechanical stirrer and a reflux condenser were introduced DMF (20OmL), l-bromo-3-tert-butylbenzene (54.3g, 0.25mol), crotyl alcohol (65mL, 0.76mol, 3eq), sodium carbonate (66.2g, 0.62mol, 2.5eq), tetrabutyl ammonium bromide (69.5g, 0.25mol, leq), palladium acetate (5.05g, 7.5mmol, 3molpercent) and tri-o-tolyl phosphine (7.6g, 25mmol, O.leq). After stirring for Ih at 90- 1000C, the reaction mixture was cooled toambient temperature. The reaction mixture was filtered over celite. The organic phase thus obtained was diluted with MTBE (50OmL) and washed three times with water (50OmL portions), dried over magnesium sulphate and concentrated. The resulting crude product was distilled with a bulb-to-bulb distillation (3mBar, 1210C) to give a colourless oil (34.7g, gc purity 73percent). The crude product was chromatographed on a silica gel column with 5percent EtOAc in hexane as elution agent giving 3-(3-fert-butylrhohenyl)butanal (12.3g, gc purity 99percent; yield 39percent).Odour: floral, aldehydic, muguet, marine.Analytical data: EPO 1H NMR (400 MHz, CHLOROFORM-d) ppm: 1.33 (d, 3H, J=5.86 Hz); 1.32 (s, 9H); 2.61-2.80 (m, 2H); 3.36 (qt, IH, J=7.16, 6.96 Hz); 7.01-7.07 (m, IH); 7.23-7.27 (m, 3H); 9.72 (t, IH, /=2.08 Hz).13C NMR (101 MHz, CHLOROFORM-^) ppm: 22.15 (q, 1C); 31.35 (q, 3C); 34.53 (d, 1C); 34.66 (s, 1C); 51.83 (t, 1C); 123.49 (d, 1C); 123.55 (d, 1C); 123.91 (d, 1C); 128.30 (d, 1C); 145.06 (s, 1C); 151.48 (s, 1C); 202.04 (d, 1C).MS: m/z (relative intensity) 204 (M+, 12), 189 (31), 171 (4), 161 (30), 147 (100), 145 (81), 130 (17), 119 (24), 117 (23), 115 (21), 105 (25), 91 (36), 77 (14), 65 (8), 57 (52), 41 (31).

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; QUEST INTERNATIONAL SERVICES B.V.; WO2008/53148; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary