Process for continuously producing 3-isothiazolinone derivatives and intermediate products thereof
AssigneeBeijing Tianqing Chemicals Co. Ltd.
InventorsYuechun Jin, Kezhong Li, Xueting Lu, Xiaolin Zhang, Yu Wang, Shuailin Zhou, Chao Li
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Abstract
The present application provides a process for continuously producing 3-isothiazolinone derivatives and intermediate products thereof, comprising continuously carrying out four steps, i.e., sulfuration, purification, amination and chlorination. Compared with the batch process of the prior art, the process of the present application may reduce the amount of manufacturing devices, lower energy consumption, simplify operations, and is therefore particularly suitable for mass production.
Claims15
A process for producing 3-isothiazolinone derivatives, comprising continuously carrying out the following four steps:
- (1) continuously adding a compound of formula I, sulfur and H2S to a first reaction device to obtain a first reaction solution comprising a compound of formula II and a compound of formula III by way of a first reaction:
- wherein the first reaction is carried out in an aqueous solution of ammonium sulfide;
- (2) continuously adding the first reaction solution and an aqueous solution of sodium sulfite to a second reaction device to obtain a second reaction solution comprising a compound of formula II by way of a second reaction:
- wherein step (2) comprises i) continuously adding a mixture of a compound of formula II and a compound of formula III and an aqueous solution of sodium sulfite to a first counter-current extraction column;
- and
- ii) continuously adding the organic phase obtained from step i) and water to a second counter-current extraction column to obtain the compound of formula II;
- (3) continuously adding the second reaction solution and a primary amine of formula IV to a third reaction device to obtain a compound of formula V by way of a third reaction:
- wherein R represents C1-C18 alkyl or C3-C18 cycloalkyl;
- and
- (4) continuously adding the compound of formula V and chlorine to a fourth reaction device to obtain a compound of formula VI by way of a fourth reaction:
- R represents C1-C18 alkyl or C3-C18 cycloalkyl, and R1 and R2 independently represent H or chlorine, and
- the fourth reaction is carried out in the presence of an ester.
Dependencies are inferred from the claim text.