Reference of 2944-49-2,Some common heterocyclic compound, 2944-49-2, name is 1-Methoxy-2,3-dimethylbenzene, molecular formula is C9H12O, 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.
A solution of 2,3-dimethylanisole (10.00 g, 73.4 mmol) in acetonitrile (500 ml) was added to a mixture of copper(II) sulphate pentahydrate (18.14 g, 72.7 mmol) and potassium peroxodisulphate (59.81 g, 0.22 mol) in water (700 ml) and heated for 30 min at reflux. After cooling, water (100 ml) and dichloromethane (150 ml) were added and the phases were separated. The aqueous phase was extracted with dichloromethane (2×200 ml). The combined organic phases were dried over anhydrous sodium sulphate, filtered and concentrated on a rotary evaporator. 4:1 n-heptane/ ethyl acetate (200 ml) was added to the brown oil and this was filtered over silica gel. The filtrate was concentrated on a rotary evaporator. 4.63 g (30.8 mmol; 42%) of a gradually crystallizing yellowish oil was obtained.1H-NMR (CDCl3, 400 MHz): delta=10.63 (s, 1H; HC?O), 7.37 (t, 1H; J=8.0 Hz; Ar-H), 6.80 (m, 2H; Ar-H), 3.88 (s, 3H; O-CH3), 2.56 (s, 3H; Ar-CH3).13C-NMR (CDCl3, 100.6 MHz): delta=192.2 (C?O), 163.0 (Ar-C), 141.9 (Ar-C), 134.4 (Ar-CH), 123.9 (Ar-CH), 123.1 (Ar-C), 108.9 (Ar-CH), 55.6 (O-CH3), 21.4 (CH3).
The synthetic route of 2944-49-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Ivoclar Vivadent AG; Moszner, Norbert; Hendrik, John; Lamparth, Iris; Barner-Kowollik, Christopher; Krappitz, Tim; Feist, Fiorian; (14 pag.)US2020/79888; (2020); A1;,
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