![](/CAS/GIF/36404-30-5.gif)
3,4-DICHLOROANISOLE synthesis
- Product Name:3,4-DICHLOROANISOLE
- CAS Number:36404-30-5
- Molecular formula:C7H6Cl2O
- Molecular Weight:177.03
Yield: 85%
Reaction Conditions:
with dimanganese decacarbonyl at 180; for 1 h;
Steps:
1,2-Dichloro-4-methoxybenzene.
General procedure: General procedure for the alkylation of phenols with dimethyl carbonate. A 17-mL stainless steel high-pressure micro reactor was charged with 3 mmol of Mn2(CO)10, W(CO)6, or Co2(CO)8, 100 mmol of the corresponding phenol, and 300 mmol of dimethyl carbonate, and the reactor was hermetically closed and heated for 1 h at 180°C. The reactor was then cooled to room temperature and opened, and the mixture was filtered through a layer of alumina. Unreacted dimethyl carbonate was distilled off, and the residue was distilled under atmospheric or reduced pressure or recrystallized from ethanol. 1,2-Dichloro-4-methoxybenzene. Yield 85%, bp 88-89°C (7 mm). 13C NMR spectrum, δC, ppm: 56.94 (OCH3), 114.69 (C5), 115.53 (C3), 124.49 (C1), 131.33 (C6), 131.62 (C2), 158.52 (C4). Found, %: C 47.25; H 3.39; Cl 39.95. C7H6Cl2O. Calculated, %: C 47.49; H 3.42; Cl 40.05.
References:
Khusnutdinov;Shchadneva;Mayakova, Yu. Yu. [Russian Journal of Organic Chemistry,2015,vol. 51,# 3,p. 330 - 334][Methylation of Phenol and Its Derivatives with Dimethyl Carbonate in the Presence of Mn2(CO)10, W(CO)6, and Co2(CO)8,2015,vol. 51,# 3,p. 330 - 334,5]
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