- Synthesis process of 2-amino-4-acetylaminoanisole
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The invention discloses a synthesis process of 2-amino-4-acetylaminoanisole. The process includes: taking 2, 4-dinitroanisole as the raw material, performing hydrogenation to obtain 2, 4-diaminoanisole, complexing the 2-amino of 2, 4-diaminoanisole with an acidification reagent, then carrying out acylation reaction with an acetylation reagent to obtain 2-amino-4-acetylaminoanisole. The synthesis method provided by the invention not only effectively reduces the oxidation of diamino and secondary acylation of amino, improves the purity and yield of 2-amino-4-acetylaminoanisole, but also recyclesthe catalyst and methanol, and effectively utilizes the hydrogenation reaction heat, meets the requirements of clean production, and can be used for industrial production.
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- A supercritical CO2For vinylsulfonyl reactive disperse dyes and its preparation method and application (by machine translation)
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The invention belongs to the field of dye synthesis, relates to a supercritical CO2 For vinylsulfonyl reactive disperse dyes, and method for preparing the compound. The compounds of this invention with the structure as shown in formula I: type definition of each group in the specification. The compounds have a relatively good dying activity, can be used for the supercritical carbon dioxide, to the wool fiber and polyester fiber has good dyeing properties. (by machine translation)
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Paragraph 0042; 0045
(2017/08/28)
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- A 3 - (N, N - disubstituted) amino acetophenone compound of clean production method
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The invention relates to a clean production method of 3-(N,N-di-substituted)aminoacetanilide compounds (III). The method comprises the following steps: (1) adding water to a compound of Formula (I), stirring uniformly, adding alkali to regulate the pH value to 6-7 when the substituent group R1 is hydrogen or not regulating the pH value when the substituent group R1 is methoxy group, adding a compound of Formula (II) and an acid-binding agent, and reacting to the end point while controlling the pH value at 4-9 and the temperature at 60-130 DEG C; (2) separating out a compound (III) to obtain a chloride salt-containing mother solution; (3) decolorizing the chloride salt-containing mother solution by using activated carbon or by adsorbing organic matters with a resin, thereby obtaining a colorless chloride salt mother solution; and (4) recovering the chloride salt from the colorless chloride salt mother solution by MVR (mechanical vapor recompression) high-efficiency concentration cooling crystallization or multiple-effect evaporation system concentration crystallization, wherein the concentration condensation water and crystallization mother solution are respectively recycled. The method lowers the production cost, and implements resource recovery and reduction on wastewater.
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Paragraph 0039-0041; 0046-0049
(2017/08/31)
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- Mutagenicity of two 2-phenylbenzotriazole derivatives, 2-[2-(acetylamino)-4-(diethylamino)-5-methoxyphenyl]-5-amino- 7-bromo-4-chloro-2H-benzotriazole and 2-[2-(acetylamino)-4-(diallylamino)-5-methoxyphenyl]-5-amino-7-bromo-4-chloro-2H-benzotriazole and their detection in river water in Japan.
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We recently detected five 2-phenylbenzotriazole (PBTA)-type mutagens (PBTA-1, PBTA-2, PBTA-3, PBTA-4 and PBTA-6) in concentrates from several rivers that flow in geographically different areas in Japan containing textile-related industries. On the basis of synthesis studies, these five PBTA derivatives were deduced to have originated from the corresponding dinitrophenylazo dyes, which are industrial chemicals used in textile dyeing, via reduction and chlorination. 2-[(2-Bromo-4,6-dinitrophenyl)azo]-5-(diethylamino)-4-methoxyacetanilide (Color Index name Disperse Blue 291, CAS registry no. 56548-64-2) and 2-[(2-bromo-4,6-dinitrophenyl)azo]-5-(diallylamino)-4-methoxyacetanilide (Color Index name Disperse Blue 373, CAS registry no. 51868-46-3) are used in textile dyeing and have 2-[(2-bromo-4,6-dinitrophenyl)azo]-4-methoxyacetanilide moieties in their structures, which are thought to be essential for their conversion to mutagenic PBTA derivatives. In the present study we have synthesized 2-[2-(acetyl-amino)-4-(diethylamino)-5-methoxyphenyl]-5-amino-7-bromo-4-chloro-2H-benzotriazole (PBTA-7) and 2-[2-(acetylamino)-4-(diallylamino)-5-methoxyphenyl]-5-amino-7-bromo-4-chloro-2H-benzotriazole (PBTA-8) from Disperse Blue 291 and Disperse Blue 373, respectively, by reduction with iron powder and subsequent chlorination with sodium hypochlorite. Both PBTA-7 and PBTA-8 exerted strong mutagenicity in Salmonella typhimurium TA98 and YG1024 in the presence of S9 mix (43 000 and 1 430 000 revertants/nmol for PBTA-7 and 40 700 and 2 213 000 revertants/nmol for PBTA-8 in TA98 and YG1024). To clarify whether PBTA-7 and PBTA-8 exist in the environment, water samples were collected at seven sites in six rivers flowing through two different regions where textile dyeing industries are located. All water samples were mutagenic in Salmonella typhimurium YG1024 with S9 mix and their potencies ranged from 108 000 to 1 990 000 revertants/g blue rayon. PBTA-7 and PBTA-8 were detected in water samples from both regions at levels of 0.1-101.4 ng/g blue rayon and 0.1-48.9 ng/g blue rayon, respectively. In some samples PBTA-7 and PBTA-8 could contribute up to 15% of the water mutagenicity.
- Watanabe, Tetsushi,Shiozawa, Tatsushi,Takahashi, Yoshifumi,Takahashi, Tomoyuki,Terao, Yoshiyasu,Nukaya, Haruo,Takamura, Takeji,Sawanishi, Hiroyuki,Ohe, Takeshi,Hirayama, Teruhisa,Wakabayashi, Keiji
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p. 293 - 299
(2008/04/18)
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