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With hydrogenchloride; sodium nitrite; In 1-methyl-pyrrolidin-2-one; water; at 50 - 70℃;
Manufacture of benzothioxanthene dye; A solution of 63.2 g 2-aminothiophenol in 400 ml NMP was combined with 20.5 g powderous sodium hydroxide and the mixture was stirred under nitrogen atmosphere for 1 hour at 60 °C. Then, a solution of 154.6 g 3-bromobenzanthrone (above Samples A, B, C or D) in 850 g NMP was added and the condensation reaction completed by stirring for two hours at 80 °C. Then, 58 g water and 51.75 g sodium nitrite were added and 75.4 g of 32 percent (w/w) hydrochloric acid were metered in at 50 °C. The mixture was stirred for 3 hours at 70 °C to complete cyclization, cooled down to 5 °C, filtered and the presscake washed with 700 g of NMP and 2 l of water. In the case of Samples C and D, this final washing step with NMP and water was repeated twice. After drying at 110 °C 132 g of C.I. Solvent Orange 63 were obtained. Content of organic bromine (determined experimentally by liquid chromatography of ions, DIN EN ISO 10304-1): Solvent Orange 63 from Sample A: 0.06 percent organic BrSolvent Orange 63 from Sample B: 0.1 percent organic BrSolvent Orange 63 from Sample C: 0.36 percent organic Br (Comparative)Solvent Orange 63 from Sample D: 1.6 percent organic Br (Comparative) It is evident that the final washing step cannot reduce the amount of brominated side-product.
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