Claims
- 1. A method for making bis-(3,5-dibromo-2-hydroxyphenyl)disulfide by heating in a reaction vessel having an inert atmosphere at about 170.degree. C to substantial completion of reaction O-(2,4,6-tribromophenyl)-N,N-dimethylthiocarbamate to give N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide, hydrolyzing the latter by heating it to reflux in methanol containing excess sodium hydroxide for a time sufficient to form bis-(3,5-dibromo-2-hydroxyphenyl)disulfide and recovering the latter from the reaction medium; or making 2,4-diiodo-6-mercaptophenol by heating in a reaction vessel having an inert atmosphere at about 195.degree. C to substantial completion of reaction O-(2,4,6-triiodophenyl)-N,N-dimethylthiocarbamate to give N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide, hydrolyzing the latter by heating it at reflux in methanol containing excess sodium hydroxide for a time sufficient to form 2,4-diiodo-6-mercaptophenol and recovering the latter from the reaction medium.
- 2. The method of claim 1 for making bis-(3,5-dibromo-2-hydroxyphenyl)disulfide by heating in a reaction vessel having an inert atmosphere at about 170.degree. C to substantial completion of reaction O-(2,4,6-tribromophenyl)-N,N-dimethylthiocarbamate to give N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide, hydrolyzing the latter by heating it to reflux in methanol containing excess sodium hydroxide for a time sufficient to form bis-(3,5-dibromo-2-hydroxyphenyl)disulfide and recovering the latter from the reaction medium.
- 3. The method of claim 1 for making 2,4-diiodo-6-mercaptophenol by heating in a reaction vessel having an inert atmosphere at about 195.degree. C to substantial completion of reaction O-(2,4,6-triiodophenyl)-N,N-dimethylthiocarbamate to give N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide, hydrolyzing the latter by heating it at reflux in methanol containing excess sodium hydroxide for a time sufficient to form 2,4-diiodo-6-mercaptophenol and recovering the latter from the reaction medium.
- 4. The method for making N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide by heating O-(2,4,6-tribromophenyl)-N,N-dimethylthiocarbamate in a reaction vessel under an inert atmosphere at about 170.degree. C to substantial completion of the reaction and recovering N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide.
- 5. The method for making N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide by heating in a reaction vessel under an inert atmosphere at a temperature of about 195.degree. C O-(2,4,6-triiodophenyl)-N,N-dimethylthiocarbamate to substantial completion of reaction and recovering N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide.
- 6. A compound of the group consisting of N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide and N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide.
- 7. The compound of claim 6 which is N-(5,7-dibromo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium bromide.
- 8. The compound of claim 6 which is N-(5,7-diiodo-1,3-benzoxathiol-2-ylidene)-N-methylmethanaminium iodide.
REFERENCE TO CO-PENDING APPLICATION
This application is a continuation-in-part of Ser. No. 686,183 filed May 13, 1976, now abandoned.
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3433803 |
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3476791 |
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823,251 |
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Continuation in Parts (1)
|
Number |
Date |
Country |
Parent |
686183 |
May 1976 |
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