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1,5-Dichloro-2-methyl-4-nitrobenzene synthesis

3synthesis methods
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Yield:7149-77-1 91%

Reaction Conditions:

with HNO3 in 1,2-dichloro-ethane at 30 - 35; for 2 h;Temperature;Reagent/catalyst;

Steps:

4-5; 2 Example 5:Preparation method of dichlorotoluene nitrate intermediate (preparation of 2,4-dichloro-5-nitrotoluene),The difference from Example 4 is that it is prepared through the following steps:

Step 1. Dissolve 32.2g (0.2mol) of 2,4-dichlorotoluene in 100g of dichloroethane in a three-necked flask,Slowly add 13.9g (0.22mol) of 98% nitric acid at 30°C and keep the temperature of the reaction system not exceeding 35°C.After the dropwise addition was completed, the reflux reaction was performed for 2.0 hours, monitored by TLC, and after the reaction was completed, a dichloroethane solution of 2,4-dichloro-5-nitrotoluene was obtained.Step 2: Add a saturated sodium bicarbonate aqueous solution to the above solution for cleaning and neutralization, and dichloroethane is distilled out.After cooling and crystallizing and drying, 37.5 g of yellow solid: 2,4-dichloro-5-nitrotoluene was obtained, and the yield was 91%.

References:

CN112266326,2021,A Location in patent:Sheet 0040-0044; 0054; 0060-0061; 0065