Purification of High-Purity 2-Mercaptobenzothiazole by Two-Steps
- 1 January 2021
- journal article
- research article
- Published by The Japan Institute of Heterocyclic Chemistry in HETEROCYCLES
- Vol. 102 (5), 851-859
- https://doi.org/10.3987/com-20-14390
Abstract
High-purity 2-mercaptobenzothiazole (2-MBT) is prepared from crude 2-MBT by aniline method under high pressure by solvent crystallization and deep impurity removal. For the first step of toluene purification, the semi-finished 2-MBT with excellent purity and yield can be obtained when the temperature of toluene solution reaches 100 degrees C and the content of toluene is about 1.5 times of that of crude 2-MBT. For the second step of deep purification, the by-products of semi-finished 2-MBT could be further removed by Na2SO3 when the mass ratio of water, the 2-MBT and Na2SO3 is 2: 1: 0.12 and the reaction condition is under 100 degrees C for 0.75 h. As a result, the purity and yield of 2-MBT can reach 99.9% and 97.3%, respectively. The preparation of high-purity 2-MBT would further optimize the market demand and meet the quality standard requirements for the development of other pharmaceutical intermediates or fine chemicals. This strategy solves the current problem of purification 2-MBT, and develops a new process technology route for the production of high-purity 2-MBT.Keywords
This publication has 7 references indexed in Scilit:
- A grand product design model for crystallization solvent designComputers & Chemical Engineering, 2020
- Sustainable rubbers and rubber additivesJournal of Applied Polymer Science, 2017
- Thermodynamic functions for solubility of 2-mercaptobenzothiazole in eleven pure organic solvents at temperatures from 273.15 K to 318.15 K and mixing properties of solutionsThe Journal of Chemical Thermodynamics, 2017
- Efficient, Iron-Catalyzed Synthesis of 2-Mercaptobenzothiazole Through S-Arylation/Heterocyclization of 2-Haloaniline with Potassium XanthateSynthetic Communications, 2015
- Synthesis and Antimicrobial Activity of a New Class of Sulfonylmethane Linked BisheterocyclesJournal of Heterocyclic Chemistry, 2014
- DBU-mediated cleavage of aryl- and heteroaryl disulfidesArkivoc, 2012
- Fly‐Ash‐Supported Synthesis of 2‐Mercaptobenzothiazole Derivatives under Microwave IrradiationSynthetic Communications, 2007