Day: October 26, 2022

On December 7, 1983, Bayer, Horst Otto; Lange, Barry Clifford; Petigara, Ramesh Balubhai published a patent.Application In Synthesis of 2-Methylisothiazol-3(2H)-one hydrochloride The title of the patent was Biocidal or biostatic compositions containing 3-isothiazolones and their uses. And the patent contained the following:

Compositions of isothiazolones I (R = R1 = H, halo, C1-4 alkyl; R2 = C1-8 alkyl, C3-6 cycloalkyl) were prepared which containing less than 15 ppm of nitrosamine and nitrosamine precursors as impurities. Thus, MeO2CCH2CH2SSCH2CH2CO2Me was amidated with MeNH2 to give 100% MeNHCOCH2CH2SSCH2CH2CONHMe (II) containing 5000 ppm MeNHCH2CH2CONH2 (III). II was recrystallized from PrOH to give II containing 0 ppm. III. II was cyclized by chlorination and Mg(NO3)2 added to the products to give a composition containing 10.3% by weight 5-chloro-2-methyl-4-isothiazolin-3-one, 5.0% by weight 2-methyl-4-isothiazolin-3-one, and 0 ppm nitrosamine and no nitrosamine precursor. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Application In Synthesis of 2-Methylisothiazol-3(2H)-one hydrochloride

The Article related to isothiazolinone nitrosamine free, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Application In Synthesis of 2-Methylisothiazol-3(2H)-one hydrochloride

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On May 24, 2017, Li, Xiaobin; Wang, Jianguo; Wang, Xinhai; Liu, Liming published a patent.Computed Properties of 26172-54-3 The title of the patent was Preparation method of high-purity 2-alkyl-4-isothiazolin-3-one. And the patent contained the following:

A process for preparation of high-purity 2-alkyl-4-isothiazolin-3-one is disclosed. The process comprises reaction of N,N’-dimethyl-3,3′-dithiodipropionamide with hydrogen chloride to obtain 2-methyl-4-isothiazolin-3-one hydrochloride salt, then washed with Et acetate, dissolving in water and neutralized with sodium carbonate to generate the product. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Computed Properties of 26172-54-3

The Article related to alkyl isothiazolinone preparation, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Computed Properties of 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On December 22, 2020, Gu, Zhenpeng; Yang, Zhaohui; Zhang, Xiaona; Zhao, Lin; Liu, Wei; Chen, Qi published a patent.SDS of cas: 26172-54-3 The title of the patent was Preparation of 2-methyl-4-isothiazolin-3-one (MIT) aqueous solution by using dipolar aprotic solvent. And the patent contained the following:

The title method includes (1) mixing 3,3′-dithiobis(N-methylpropionamide) or 3-mercapto-N-methylpropanamide with solvent, and adding halogenating agent (chlorine gas, sulfuryl chloride, etc.) for a halogenation ring-closing reaction. (2) Filtering to obtain a product, washing the filter cake with Et acetate, and drying to obtain 2-methyl-4-isothiazolin-3-one hydrochloride solid. (3) Dissolving with a sodium carbonate aqueous solution to obtain an aqueous solution having pH of 5.0-7.0 and the mass content of 2-methyl-4-isothiazolin-3-one of 50%. The solvent comprises chlorination solvent (dichloromethane, chloroform, etc.) and dipolar aprotic solvent (acetonitrile, DMF, etc.). The prepared 2-methyl-4-isothiazolin-3-one has the purity up to above 99.9% and the content of 5-chloro-2-methyl-4-isothiazolin-3-one controlled at below 100 ppm. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).SDS of cas: 26172-54-3

The Article related to methyl isothiazolinone preparation, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.SDS of cas: 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On January 1, 2007, Cuixart Grande, Jesus Maria published a patent.Quality Control of 2-Methylisothiazol-3(2H)-one hydrochloride The title of the patent was Procedure for preparing 2-alkylisothiazolones and their formulation in stable form alone or in association to other molecules with biocidal activity. And the patent contained the following:

This invention relates to a procedure for preparing 2-alkylisothiazolones of formula I and their formulations in stable forms alone or in association to other mols. with biocidal activity. 2-Alkylisothiazolones may be used as industrial biocides. A procedure for preparing compounds of formula I wherein R is C1-8 alkyl; X and X1 are independently H and Cl; are claimed. These compounds were obtained by cyclization of 3,3′-dithiopropionamides. Several example on formulations of these compounds are also provided. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Quality Control of 2-Methylisothiazol-3(2H)-one hydrochloride

The Article related to alkylisothiazolone preparation formulation, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Quality Control of 2-Methylisothiazol-3(2H)-one hydrochloride

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On January 21, 2009, Li, Shaotong published a patent.SDS of cas: 26172-54-3 The title of the patent was Method for synthesizing alkyl isothiazolone hydrochloride by chlorination-cyclization of alkyl dithiodipropionamide with chlorine and sulfuryl chloride. And the patent contained the following:

The invention relates to a method for synthesizing alkyl isothiazolone hydrochloride by chlorination-cyclization of alkyl dithiodipropionamide or alkyl thiopropionamide with chlorine and sulfuryl chloride. The method has advantages of simple operation, low cost and high conversion rate. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).SDS of cas: 26172-54-3

The Article related to thiazolone methyl hydrochloride preparation, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.SDS of cas: 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On April 6, 2011, Jiang, Zhikai; Jiang, Yifan published a patent.Electric Literature of 26172-54-3 The title of the patent was A process for preparing isothiazolone derivatives. And the patent contained the following:

The invention relates to a process for the preparation of isothiazolone derivatives I or II, wherein R1 is H, alkyl, cycloalkyl, or (un)substituted aryl; R2 and R3 independently = H or Cl. For instance, 1,2-benzisothiazol-3(2H)-one was prepared from 2-mercapto-benzonitrile in the presence of Cl2 in 82.28% yield. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Electric Literature of 26172-54-3

The Article related to isothiazolone derivative preparation heterocyclization, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Electric Literature of 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

Weiler, E. D.; Miller, G. A.; Hausman, M. published an article in 1976, the title of the article was Isothiazoles. VIII: isothiazolidin-3-one derivatives.Category: isothiazole And the article contains the following content:

The isothiazolidinone I (R = R1 = Me) was prepared by cyclization of (MeNHCOCHMeCH2)2S2 in EtOAc in the presence of Cl and I (R, R1 given: Me, Cl; Bu, Me; Bu, Cl; CH2Ph, Cl; CH2C6H3Cl2-3,4, Cl) were obtained by the addition of Cl to the appropriate isothiazolinones II. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Category: isothiazole

The Article related to isothiazolidinone trichloro, thiazolinone addition chlorine, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Category: isothiazole

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On June 17, 1992, Petigara, Ramesh Balubhai; Horton, Isaac Byron published a patent.Computed Properties of 26172-54-3 The title of the patent was Process for preparing 3-isothiazolone compounds. And the patent contained the following:

A process for the preparation of salt-free, and optionally water-free, isothiazolones comprising treating a solution of an acid salt of an isothiazolone with a basic anion exchange resin, preferably a weak base anion exchange resin, and separating the free base isothiazolone solution from the spent resin is claimed. Five different ion exchange resins were evaluated: two strong base anion exchange resins (Amberlite IRA-9OOC-OH and IRA-420C-OH) and 3 weak base anion exchange resins (Amberlite IRA-68, Amberlyst A21 and Diaion WA-30) were used. Thus, chlorination of N-methyl-3-mercaptopropionamide in EtOAc gave a mixture of HCl salts of 5-chloro-2-methyl-3-isothiazolinone and 2-methyl-3-isothiazolone which were neutralized with the described resins. The resultant salt-free isothiazolones are useful as microbicides in environments where even low concentrations of metal salts are undesirable, for example, latex emulsions and corrosion sensitive aqueous systems. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Computed Properties of 26172-54-3

The Article related to isothiazolone hydrochloride salt preparation neutralization resin, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Computed Properties of 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On October 25, 1995, Petigara, Ramesh Balubbai published a patent.Synthetic Route of 26172-54-3 The title of the patent was Purification of 3-isothiazolones. And the patent contained the following:

The title process for producing substantially separated 5-chloro-2-methyl-3-isothiazolone (CMI) and 2-methyl-3-isothiazolone (MI) from a mixture of their hydrochloride salts comprises heating a mixture of CMI.HCI and MI.HCI in an org, solvent for a period of time necessary to fully dissociate CMI.HCI but insufficient to fully dissociate MI.HCI. CMI free base dissolves in the solvent and the products may recovered by filtration. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Synthetic Route of 26172-54-3

The Article related to chloromethylisothiazolone purification, methylisothiazolone purification, Heterocyclic Compounds (More Than One Hetero Atom): Thiazoles, Isothiazoles and other aspects.Synthetic Route of 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com

On November 26, 1992, Hahn, Soon Jong; Kim, Jin Man; Park, Young published a patent.Synthetic Route of 26172-54-3 The title of the patent was Preparation of N-alkyl-4-isothiazolin-3-ones from dithiodipropionamides and sulfuryl halides. And the patent contained the following:

Title compounds [I; R1 = Me, Me(CH2)7; R2 = H, Cl], were prepared by (1) treatment of (SCH2CH2CO2H)2 with SOCl2 to give (SCH2CH2COCl)2, (2) treatment of the latter with R1NH2 to give (SCH2CH2CONHR1)2, and (3) treatment of this with SO2X2 (X = halo) in an organic solvent. Thus, [SCH2CH2CONH(CH2)7Me]2 was treated with SO2Cl2 in CH2Cl2 at 0-25° to give 90.5% title compound II. The experimental process involved the reaction of 2-Methylisothiazol-3(2H)-one hydrochloride(cas: 26172-54-3).Synthetic Route of 26172-54-3

The Article related to dithiodipropionamide sulfuryl halide cyclocondensation alkylisothiazolinone, cyclocondensation reaction and other aspects.Synthetic Route of 26172-54-3

Referemce:
Isothiazole – Wikipedia,
Isothiazole – ScienceDirect.com