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    • 96. 发明专利
    • Production of lignan
    • 生产LIGNAN
    • JPS6118734A
    • 1986-01-27
    • JP13913484
    • 1984-07-06
    • Tsumura Juntendo Inc
    • TOBINAGA KIYOTERUTAKEYA TETSUYA
    • C07C5/44C07C1/00C07C13/547C07C15/50C07C33/26C07C41/00C07C41/18C07C43/21C07C43/215C07C43/23C07C67/00C07D317/64C07D493/04
    • PURPOSE: The dimerization of trimethoxyphenyl-2-propanone is followed by reaction with ethyl orthoformate and benzoic acid, then reduction and cyclization, to enable high yield production of benzocyclo-octadiene type lignan which is used as an improver of hepatic disorders.
      CONSTITUTION: A compound of formula I (R
      1 WR
      3 are lower alkyl, lower alkoxy or R
      1 and R
      2 incorporate to form methylenedioxy, ethylenedioxy; R
      4 is lower alkyl) to give a dimer of formula II. Then, the product is allowed to react with ethyl orthoformate and benzoic acid at 100W200°C and the reaction mixture is extracted with a halogen-containing organic solvent, dried and the solvent is removed. The resultant residue is recrystallized from a lower alcohol to give a trans-alkene of formula III, while cis-alkene is obtained from the mother liquor. Then, individual isomers are separately reduced and cyclized using a composition for oxidation containing ferric perchlorate and ferric chloride dissolved in acetic anhydride and acetonitrile to give the objective compounds of formula V or VI.
      COPYRIGHT: (C)1986,JPO&Japio
    • 目的:三甲氧基苯基-2-丙酮的二聚反应接着与原甲酸乙酯和苯甲酸反应,然后还原和环化,以使苯并环辛二烯型木脂素高产量生产,用作肝脏疾病的改良剂。 构成:式I化合物(R 1 -R 3是低级烷基,低级烷氧基或R 1和R 2结合形成亚甲二氧基,亚乙二氧基; R 4是低级烷基),得到式Ⅱ二聚体。 然后,使产物与100-200℃的原甲酸乙酯和苯甲酸反应,反应混合物用含卤素的有机溶剂萃取,干燥并除去溶剂。 所得残余物从低级醇中重结晶,得到式III的反式烯烃,而从母液获得顺式 - 烯烃。 然后,使用溶解在乙酸酐和乙腈中的含有高氯酸铁和氯化铁的氧化组合物分别还原和环化单个异构体,得到式V或VI的目标化合物。
    • 98. 发明专利
    • 1,1-diarylalkane derivative
    • 1,1-DIARYLALKANE DERIVATIVE
    • JPS59196832A
    • 1984-11-08
    • JP7078783
    • 1983-04-21
    • Nippon Petrochem Co Ltd
    • SATOU ATSUSHIKAWAKAMI SHIGENOBUDOI HIDEYUKI
    • C08F12/00C07C1/00C07C15/50C07C67/00C08F12/06C08F12/32H01B3/22
    • NEW MATERIAL:The compound of formula I (R
      1 is H or CH
      3 ; R
      2 and R
      4 are H or 1W4C alkyl; R
      3 is 1W4C alkyl).
      EXAMPLE: 1-Phenyl-1-(4'-vinylphenyl)ethane.
      USE: An intermediate capable of easily producing a polymer readily crosslinkable with radiation, by radical or cationic polymerization. The above polymer crosslinked with radiation has extremely high heat resistance, and is useful as an electrical insulation oil.
      PREPARATION: The compound of formula V (an example of the formula I ) can be prepared by (1) reacting the compound of formula II with acetyl chloride in the presence of a Friedel-Crafts catalyst such as aluminum chloride, (2) reacting the resultant ketone of formula III with a reducing agent such as sodium borohydride to selectively reduce the acetyl group, and (3) dehydrating the obtained alcohol of formula IV with a dehydration agent such as potassium bisulfate, etc.
      COPYRIGHT: (C)1984,JPO&Japio
    • 新材料:式Ⅰ化合物(R1为H或CH3; R2和R4为H或1-4C烷基; R3为1-4C烷基)。 实施例:1-苯基-1-(4'-乙烯基苯基)乙烷。 用途:通过自由基或阳离子聚合,能够容易地制备易于与辐射交联的聚合物的中间体。 上述与辐射交联的聚合物具有极高的耐热性,并且可用作电绝缘油。 制备:式V化合物(式I的实例)可以通过以下步骤制备:(1)在Friedel-Crafts催化剂如氯化铝存在下使式II化合物与乙酰氯反应,(2)使 得到式III的酮与还原剂如硼氢化钠反应以选择性还原乙酰基,和(3)用脱硫剂如硫酸氢钾等将得到的式IV的醇脱水。
    • 99. 发明专利
    • Dimerization of alpha-methylstyrene
    • 二甲基苯乙烯的二聚体
    • JPS59190927A
    • 1984-10-29
    • JP6591583
    • 1983-04-14
    • Nippon Petrochem Co Ltd
    • GOTOU MASATOMATSUMURA YASUODOI HIDEYUKI
    • C07C2/26B01J21/00B01J21/16C07B61/00C07C1/00C07C15/50C07C67/00
    • Y02P20/52
    • PURPOSE: In dimerizing the titled compound using activated clay or acid clay as a catalyst, to obtain an unsaturated linear dimer of the titled compound useful as a raw material for a lubricating oil of traction drive in high yield, by making Cellosolve exist in the reaction system.
      CONSTITUTION: In dimerizing α-methylstyrene using activated clay or acid clay as a catalyst, 2W40times, preferably 5W20times as much Cellosolve, preferably ≤6C Cellosolve as the catalyst by weight is added to the reaction system, to prevent the catalyst from blocking, formation of high-boiling substances is suppressed, to give an unsaturated linear dimer of α-methylstyrene, especially 2,4- diphenyl-4-methylpentene-1 useful as a polymerization adjustor in high yield. This process has merits wherein amounts of the catalyst and the coexisting substance used are small. The reaction temperature is 40W150°C, preferably 50W 120°C.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:使用活性粘土或酸性粘土作为催化剂使标题化合物二聚,得到标题化合物的不饱和线性二聚体,其用作牵引驱动用润滑油的高产率原料,通过使溶胶存在于反应中 系统。 构成:在使用活性粘土或酸性粘土作为催化剂使α-甲基苯乙烯二聚的过程中,加入到反应体系中的2-40倍,优选5-20倍的溶纤剂,优选<= 6C溶媒作为催化剂,以防止催化剂 抑制高沸点物质的形成被抑制,得到α-甲基苯乙烯的不饱和线性二聚体,特别是可用作聚合调节剂的2,4-二苯基-4-甲基戊烯-1。 该方法的优点在于其中使用的催化剂和共存物质的量少。 反应温度为40-150℃,优选为50-120℃。