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Method for preparing N-tertiary butyl benzothiazole sulfonamide

A technology of thiazole sulfenamide and benzothiazole, applied in organic chemistry and other fields

Active Publication Date: 2010-03-24
SINOPEC NANJING RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the shortcomings of the above synthetic methods, the present invention proposes a synthetic process for NS, which can effectively solve the problems existing in the existing synthetic methods, stabilize the product yield above 95%, and have a melting point of 105°C

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0010] In the 250ml four-neck flask with stirrer, thermometer, reflux condenser, add 80 milliliters of water, 0.1 gram of non-ionic surfactant agricultural milk 600#, open stirring, add 17g (0.1mol) gram to promote in batches at room temperature Add agent M, stir for half an hour after adding tert-butylamine, then add 12 grams (0.15mol) of tert-butylamine, control the addition temperature at 30-35°C, add time for 20-30 minutes, maintain at 30-35°C for 2 hours after adding tert-butylamine, maintain Complete, at 35-40°C, add 60 ml of 10% sodium hypochlorite in 1-4 hours, after adding sodium hypochlorite, raise the temperature to 60-65°C and continue to maintain for 1 hour, add 2 ml of 5% sodium sulfite solution, stir and cool down to 15- 20°C, filter, wash four times with 40 ml of water, the first washing water and the mother liquor are combined and distilled to recover tert-butylamine, the last washing water is 50°C hot water, apply it as the dilution water of the next batch, fi...

Embodiment 2

[0012] The operating conditions were the same as in Example 1, except that 0.1 g of ionic surfactant was used instead of Nongru 600# to obtain 23.2 g of finished product with a melting point of 105° C. and a NS yield of 97.5%. Methanol insoluble matter 0.52%.

Embodiment 3

[0014] The operating conditions were the same as in Example 1, but 0.1 g of polyoxyethylene octadecylamine was used instead of Nongru 600# to obtain 23.1 g of finished product with a melting point of 105.1° C., a NS yield of 97%, and methanol insolubles of 0.3%.

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PUM

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Abstract

The invention relates to a method for preparing N-tertiary butyl benzothiazole sulfonamide, belonging to the field of fine chemical engineering. In the method, 2-thiol group benzothiazole crude product and tert-butylamine are used as raw materials, with the existence of surfactant, sodium hypochlorite is taken as oxidant for oxidation reaction, after completing the reaction proper amount of antioxidant is added, and excessive unreacted sodium hypochlorite is removed, thus stability of the product in the drying process is improved. The invention dispenses with consumption of sulphuric acid andsodium hydroxide, therefore waste water amount is small, product yield can be over 95%, consumption of main raw materials is low, thus the invention is suitable for industrial production.

Description

technical field [0001] The invention specifically relates to a method for preparing N-tert-butylbenzothiazole sulfenamide by using sodium hypochlorite as an oxidant. Background technique [0002] N-tert-butyl-2-benzothiazole sulfenamide (hereinafter referred to as accelerator NS) is one of the important varieties of sulfenamide vulcanization accelerators. It has two advantages of scorch resistance and fast vulcanization speed. In natural rubber, styrene-butadiene rubber, cis-butadiene rubber, and isoprene rubber, it is especially suitable for furnace-process carbon black rubber with high alkalinity, with slight discoloration and pollution, and can replace the carcinogenic NOBS containing secondary amino groups (N-morpholino benzothiazole sulfenamide), Germany legislated in 1994 to replace NOBS used in the tire industry with CBS (CZ) or NS. At present, the production and consumption of NS abroad account for 40% of the total amount of thiazole vulcanization chemicals. In rec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
Inventor 付春刘伊文陶建青张云刚
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD