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ChemicalBook CAS DataBase List 3,4-Dichlorotoluene

3,4-Dichlorotoluene synthesis

10synthesis methods
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Yield:-

Reaction Conditions:

with aluminum (III) chloride;chlorine;iron at 40; for 16 h;Molecular sieve;Overall yield = 90.5 %;

Steps:

3
(A) Preparation of chlorination catalyst: 8 parts of iron powder, 15 parts of aluminum trichloride and 70 parts of L-type molecular sieve were mixed, and then mixed with silica sol and then treated at 100C for 4 to 6 hours to obtain a chlorination catalyst; (B) chlorination of p-chlorotoluene: Chlorotoluene is added in the reaction kettle, the chlorination catalyst is added, the stirring is started to uniformly distribute the catalyst in the material, the chlorine gas flowmeter valve of the chlorine gas buffer tank is opened, the chlorine gas is introduced into the reaction kettle equipped with o-chlorotoluene, The reaction was carried out at a temperature of 40 ± 5 °C, and the reaction temperature was controlled at 1: 0.7. The reaction temperature was controlled to 40 ± 5 °C. The reaction of chlorination with chlorine Time control in 16 hours, stop chlorine, the exhaust gas by NaOH solution to remove the unreacted Cl2, continue stirring for 20 minutes, so that the reactor reaction of chlorine completely; (C) Separation of components: The reaction product is subjected to a m-chlorination step through a rectification column, and the unreacted raw material is first separated toluene, and then distillation of the bottom of heavy components through the benzene distillation column distillation, separation of 2,4-dichlorotoluene and3, 4-dichlorotoluene. The product yield was 90.5%, chlorine utilization rate was 93.1%, and the purity of 2,4-dichlorotoluene in the finished product was 99.9%.

References:

Nanjing Zhong Teng Chemical Co., Ltd.;Zhong, Hua;Lu, Minshan;Chen, Xiuzhen;Cai, Weizhong CN105367381, 2016, A Location in patent:Paragraph 0017-0019

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