Benzene, 2-methoxy-4,5-dimethyl-1,3-dinitro- synthesis
- Product Name:Benzene, 2-methoxy-4,5-dimethyl-1,3-dinitro-
- CAS Number:160754-06-3
- Molecular formula:C9H10N2O5
- Molecular Weight:226.19
4097-61-4
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Yield:160754-06-3 93.9%
Reaction Conditions:
with sodium carbonate in water;1,2-dichloro-ethane;
Steps:
3 Preparation of 2,6-dinitro-3,4-dimethyl anisole
EXAMPLE 3 Preparation of 2,6-dinitro-3,4-dimethyl anisole A solution of 226 g 2,6-dinitro-3,4-xylenol, 93.7%. (1 mole) in two liters 1,2-dichloroethane was placed in a three liter reaction flask. Sodium carbonate 128 g (1.2 moles) and 0.81 g Didecyldimethyl-ammonium chloride (DDAC) were added to the above solution and afterwards 151.3 (1.2 moles) of dimethylsulfate were introduced during 15 minutes at the ambient temperature. The reaction mixture was heated with stirring to reflux during two hours. Water (400 ml) was added and heating was continued for another hour. This mixture was cooled to 25° C. and allowed to separate in two phases. The lower organic phase was separated, washed with water to neutral. The solvent was next recovered by distillation and the remaining oily produce solidified by cooling. A product (225.8 g) of 94%. 2,6-dinitro-3,4-dimethylanisole was obtained at a 93.9% of the theoretical yield based on 2,6-dinitro-3,4-xylenol consumed.
References:
US5475148,1995,A
4685-47-6
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