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    • 11. 发明授权
    • Process for producing phthaloyl dichlorides of high purity
    • 生产高纯度邻苯二甲酰氯的方法
    • US4165337A
    • 1979-08-21
    • US844814
    • 1977-10-25
    • Shigeo YoshinakaMasaharu DoyaSeiji UchiyamaSadao Nozaki
    • Shigeo YoshinakaMasaharu DoyaSeiji UchiyamaSadao Nozaki
    • C07C63/15B01J19/12C07C17/14C07C51/00C07C51/60C07C67/00C07C51/58
    • C07C17/14C07C51/60
    • A batchwise or continuous process for producing isophthaloyl dichloride or terephthaloyl dichloride having a high purity which comprises, in combination, (1) a first step of producing .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene by reacting meta- or para-xylene with chlorine under the irradiation of ultraviolet-containing rays, the reaction being carried out in the presence of, as a solvent, .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene added at the outset of the reaction; (2) a second step of producing isophthaloyl dichloride or terephthaloyl dichloride by reacting the .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene obtained in the first step with isophthalic acid or terephthalic acid; and (3) a third step of purifying the isophthaloyl dichloride or terephthaloyl dichloride obtained in the second step by dissolving the isophthaloyl dichloride or terephthaloyl dichloride in 0.3 to 6 parts by weight; per part by weight of the phthaloyl dichloride, of C.sub.6 -C.sub.10 aliphatic hydrocarbon solvent, and cooling the solution to a temperature of the specified range thereby to recrystallize the phthaloyl dichloride.
    • 用于制备具有高纯度的间苯二酰二氯或对苯二甲酰氯的间歇或连续方法,其组合包括(1)通过使间位化合物反应生成α,α,α,α',α',α'-六氯代二甲苯的第一步骤, 或对二甲苯与氯在紫外线照射下反应,反应在作为溶剂的存在下进行,α,α,α,α',α',α'-六氯化碳在开始时加入 反应; (2)通过使第一步获得的α,α,α,α',α',α'-六氯二苯与间苯二甲酸或对苯二甲酸反应,生产间苯二酰二氯或对苯二甲酰氯的第二步; 和(3)通过将间苯二酰二氯或对苯二酰氯溶解在0.3至6重量份中来纯化在第二步中获得的间苯二酰二氯或对苯二甲酰氯的第三步骤; 每重量份邻苯二甲酰二氯化物,C 6 -C 10脂族烃溶剂,并将溶液冷却至指定范围的温度,从而使邻苯二甲酰氯二氯化物重结晶。
    • 12. 发明申请
    • METHOD FOR PRODUCING 3-METHYL-CYCLOPENTADECENONES, METHOD FOR PRODUCING (R)- AND (S)- MUSCONE, AND METHOD FOR PRODUCING OPTICALLY ACTIVE MUSCONE
    • 用于生产3-甲基环戊二烯的方法,用于生产(S) - 和(S) - 马铃薯的方法,以及用于生产光学活性麦克风的方法
    • US20110172465A1
    • 2011-07-14
    • US13063541
    • 2009-03-27
    • Masaharu Doya
    • Masaharu Doya
    • C07C45/61
    • C07B53/00B01J23/02B01J23/06B01J31/1805B01J31/2452B01J2531/0266B01J2531/821C07C45/62C07C45/74C07C45/82C07C49/385C07C49/587
    • By intramolecular condensation reaction of 2,15-hexadecanedione in a gaseous phase with a compound of a Group II element of the Periodic Table as a catalyst, 3-methyl-cyclopentadecenones is generated. Magnesium oxide, calcium oxide, or zinc oxide is desirable as the catalyst for the intramolecular condensation reaction. (R)- and (S)-muscone is generated by subjecting 3-methyl-cyclopentadecenones obtained as above to hydrogenation by using a catalyst. Palladium catalyst is desirable as the hydrogenation catalyst. Optically active muscone is generated by separating 3-methyl-cyclopentadecenones into respective components thereof by means of precision distillation and subsequently subjecting the separated 3-methyl-cyclopentadecenones to asymmetric hydrogenation by using an optically active ruthenium complex catalyst. The production methods described above enable easy and economical production of 3-methyl-cyclopentadecenones, (R)- and (S)-muscone, and optically active muscone.
    • 通过将气相中的2,15-十六烷二酮与周期表的II族元素的化合物作为催化剂的分子内缩合反应,产生3-甲基 - 环戊烯酮。 作为分子内缩合反应的催化剂,优选氧化镁,氧化钙或氧化锌。 通过使用上述得到的3-甲基 - 环十五烯酮通过使用催化剂进行氢化而生成(R) - 和(S) - 壳多糖。 作为氢化催化剂,钯催化剂是理想的。 通过精密蒸馏将3-甲基 - 环十五烯酮分成其各自的组分,然后通过使用光学活性钌络合物催化剂将分离的3-甲基 - 环十五烯酮进行不对称氢化,产生光学活性的肌肉。 上述制造方法能够容易且经济地生产3-甲基 - 环戊烯酮,(R) - 和(S) - 软骨素和光学活性的肌肉。
    • 13. 发明授权
    • Process for producing
.alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene
    • 制备{60,{60,{60,{60 {40,{60 {40,{60 {40-六氯二氧化碳
    • US4029560A
    • 1977-06-14
    • US671698
    • 1976-03-29
    • Shigeo YoshinakaMasaharu DoyaSeiiji UchiyamaSadao Nozaki
    • Shigeo YoshinakaMasaharu DoyaSeiiji UchiyamaSadao Nozaki
    • C07C17/00C07C17/14C07C22/04C07C51/00C07C51/60C07C63/15C07C63/30C07C67/00C08G69/32B01J1/10
    • C08G69/32C07C17/14C07C51/60Y10S204/914
    • This invention concerns to a process for .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene by reacting m-xylene or p-xylene or a partially chlorinated product thereof with chlorine under the irradiation of ultraviolet rays, the process comprising (1) a first-step chlorination reaction which is carried out in the presence of .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene as a solvent added at the initial stage of the reaction, and continued until a compound convertible to .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene by chlorination becomes substantially absent in the reaction mixture, and (2) a second-step chlorination reaction which is continued from the first-step chlorination and carried out to convert difficulty-separable by-products present in the reaction mixture to easily-separable compounds. This invention also concerns to a process for producing an aromatic dicarboxylic acid chloride which comprise reacting the resulting .alpha.,.alpha.,.alpha.,.alpha.',.alpha.',.alpha.'-hexachloroxylene with isophthalic acid or terephthalic acid.
    • 本发明涉及一种通过在紫外线照射下使间二甲苯或对二甲苯或其部分氯化产物与氯反应的α,α,α,α',α',α'-六氯二氧化碳的方法,该方法包括 (1)第一步氯化反应,其在α,α,α,α',α',α'-六氯二苯作为反应初始阶段加入的溶剂存在下进行,并持续进行到化合物 在反应混合物中通过氯化可转化成α,α,α,α',α',α'-六氯二苯基本上不存在,和(2)第二步氯化反应,继续从第一步氯化并进行 将反应混合物中存在的难以分离的副产物转化成容易分离的化合物。 本发明还涉及一种制备芳族二羧酰氯的方法,其包括使所得的α,α,α,α',α',α'-六氯代二甲苯与间苯二甲酸或对苯二甲酸反应。