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    • 3. 发明授权
    • Process for production of cresols
    • 甲酚生产工艺
    • US5399791A
    • 1995-03-21
    • US202160
    • 1994-02-25
    • Kiyoshi IkimiYoichi IkedaAkira MurakamiKazushige OkamotoTooru TokumaruMotoo Hazama
    • Kiyoshi IkimiYoichi IkedaAkira MurakamiKazushige OkamotoTooru TokumaruMotoo Hazama
    • C07C39/07C07C37/08C07C37/06
    • C07C39/07
    • There is disclosed a process for the production of cresols, including the steps of: (a) conducting oxygenation of cymene with oxygen gas or an oxygen-containing gas without any addition of an alkali, thereby obtaining a solution of oxygenation products containing tertiary and primary hydroperoxides of cymene; (b) washing the solution of oxygenation products obtained in step (a) with an aqueous alkali solution at a temperature in the range of from 10.degree. to 95.degree. C.; (c) subjecting the solution of oxygenation products obtained in step (b) to hydrogenation at a temperature in the range of from 60.degree. to 100.degree. C. to decrease the content of primary hydroperoxide in such a manner that the weight ratio of primary hydroperoxide to tertiary hydroperoxide is not greater than 1/25 (w/w); (d) subjecting the solution treated in step (c) to decomposition in the presence of a catalyst; and (e) subjecting the solution treated in step (d) to hydrogenation to obtain cresols.
    • 公开了一种生产甲酚的方法,包括以下步骤:(a)在不加碱的条件下,用氧气或含氧气体进行甲基异丙基苯的氧化反应,从而得到含有叔, 伞形氢过氧化物; (b)在10℃至95℃的温度范围内用碱水溶液洗涤步骤(a)中获得的氧合产物的溶液; (c)将步骤(b)中获得的氧合产物溶液在60℃至100℃的温度范围内进行氢化,以降低初级氢过氧化物的含量,使得初级氢过氧化物的重量比 叔氢过氧化物不大于1/25(w / w); (d)使在步骤(c)中处理的溶液在催化剂存在下进行分解; 和(e)使步骤(d)中处理的溶液进行氢化以获得甲酚。
    • 5. 发明授权
    • Process for producing aromatic amide compounds
    • 芳香族酰胺化合物的制备方法
    • US5442114A
    • 1995-08-15
    • US182460
    • 1994-01-18
    • Kan TakamineMichio YamatoAkira MurakamiTooru TokumaruYoshinori NakayamaMotoo Hazama
    • Kan TakamineMichio YamatoAkira MurakamiTooru TokumaruYoshinori NakayamaMotoo Hazama
    • C07C231/02C07C235/24
    • C07C231/02C07C235/24
    • There is disclosed a process for producing an aromatic amide compound of the general formula (4), including the steps of subjecting an o-nitrophenol compound of the general formula (1) to catalytic reduction in acetone or an aromatic hydrocarbon solvent under the presence of a nickel catalyst to give an o-aminophenol compound of the general formula (2); and (b) subjecting the o-aminophenol compound of the general formula (2) to condensation with an acid chloride compound having a sulfur content of 0.5% or less, based on the weight of the acid chloride compound, of the general formula (3) in acetone or an aromatic hydrocarbon solvent under an atmosphere of an inert gas having an oxygen concentration of 1% or less. The acid chloride compound having a sulfur content of 0.5% or less, based on the weight of the acid chloride compound, of the general formula (3) may be obtained by allowing a carboxylic acid compound of the general formula (5) to react with thionyl chloride and by concentrating the reaction mixture. Also disclosed is another process for producing an aromatic amide compound of the general formula (4), including the step of subjecting an o-aminophenol hydrochloride salt of the general formula (6) to condensation with an acid chloride compound having a sulfur content of 0.8% or less, based on the weight of the acid chloride compound, of the general formula (3) in an inert solvent.
    • 公开了通式(4)的芳香族酰胺化合物的制造方法,包括以下步骤:将通式(1)的邻硝基苯酚化合物在丙酮或芳族烃溶剂中进行催化还原, 镍催化剂,得到通式(2)的邻氨基苯酚化合物; 和(b)将通式(2)的邻氨基苯酚化合物与基于酰基氯化合物的重量的硫含量为0.5%以下的酰基氯化合物进行缩合,通式(3) )在丙酮或芳烃溶剂中,在氧浓度为1%以下的惰性气体气氛下进行。 通式(3)的酰基氯化合物的硫含量为0.5%以下的酰氯化合物可以通过使通式(5)的羧酸化合物与 亚硫酰氯,并浓缩反应混合物。 还公开了制备通式(4)的芳族酰胺化合物的另一种方法,包括使通式(6)的邻氨基苯酚盐酸盐与硫含量为0.8的酰氯化合物缩合的步骤 %以下,基于酰基氯化合物的重量,在惰性溶剂中。
    • 7. 发明授权
    • Process for producing O,O-di-lower-alkylchlorothiophosphate
    • O,O-二低级烷基氯代硫代磷酸酯的制备方法
    • US4769494A
    • 1988-09-06
    • US11009
    • 1987-02-05
    • Motomasa OhsuKoichi KamemotoManabu YahataTooru TokumaruTakeshi HiokiHiroshi Ueda
    • Motomasa OhsuKoichi KamemotoManabu YahataTooru TokumaruTakeshi HiokiHiroshi Ueda
    • C07F9/20C07F9/02
    • C07F9/20
    • A continuous process for producing O,O-di-lower alkylchlorothiophosphate very important as an intermediate for organo-phosphate series agricultural chemicals which comprises continuously reacting phosphorus sulfochloride with a lower alcohol in the presence of caustic soda according to a multi-stage reaction form comprising from 3 to 8 stages in which the following conditions are satisfied:(1) The amounts of caustic soda and a lower alcohol used shall be from 2 to 2.2 moles and 10 moles or more, respectively, based on 1 mole of phosphorus sulfochloride.(2) Caustic soda, water and the lower alcohol shall be used as a caustic soda/water/lower alcohol solution, and besides the caustic soda concentration of the aqueous caustic soda in said solution shall be from 30.0 to 99.5 wt.%.(3) To the 1st reaction stage shall be continuously supplied the whole amount of phosphorus sulfochloride required and from 45 to 85 wt.% each of the amounts of caustic soda and the lower alcohol required; and to the 2nd and subsequent reaction stages shall be continuously supplied the residual caustic soda and lower alcohol in divided portions so that the substantial amounts supplied become successively small toward the final reaction stage.(4) The temperature of the reaction system shall be -5.degree. C. or lower.(5) The residence time in the reaction system shall be within 4 hours.
    • 一种用于生产作为有机磷酸酯系农药的中间体非常重要的O,O-二低级烷基氯硫代磷酸酯的连续方法,其包括在苛性钠存在下,根据多阶段反应形式连续地使磷酰氯与低级醇反应,包括 从3到8个阶段,其中满足以下条件:(1)基于1摩尔磷酰氯,苛性钠和低级醇的用量分别为2至2.2摩尔和10摩尔或更多。 (2)苛性钠,水和低级醇应用作苛性钠/水/低级醇溶液,除了所述溶液中的苛性钠水溶液的苛性钠浓度外还应为30.0至99.5重量%。 (3)向第一反应阶段连续供应所需的全部硫磺磷酸盐和每一种苛性钠和所需的低级醇的45至85重量%; 并且连续向第二和随后的反应阶段连续地供应残留的苛性钠和低级醇,使得所供应的实质量向着最终反应阶段依次小。 (4)反应体系的温度应在-5℃以下。 (5)反应体系中的停留时间应在4小时内。