INDENE COMPOUND AND PRODUCTION OF ITS DERIVATIVE

    公开(公告)号:JPH08325211A

    公开(公告)日:1996-12-10

    申请号:JP13163195

    申请日:1995-05-30

    Applicant: TEIJIN LTD

    Abstract: PURPOSE: To efficiently obtain an indene derivative expressed by a specific formula and useful as a synthetic intermediate for CD ring part in simple synthesis of 1α,25-dihydroxyvitamine D3 in a short process. CONSTITUTION: This derivative is expressed by formula I [R is H, a 2-8C acyl or a tri(1-6C hydrocarbon)-substituted silyl, e.g. (6R)-6-[(4S, 7aS)-4-benzoyloxy-7a- methylinden-1-yl]-2-nitro-3-heptanol. Furthermore, the compound is preferably obtained by reacting a compound of formula II in the presence of a basic catalyst such as triethylamine in an organic solvent such as nitroethane or tetrahydrofuran or a mixed solvent of an organic solvent with water at 0 deg.C to ambient temperature. The compound of formula I is used as a raw material and successively reacted and converted into a compound of formula III, which is then reacted with a methylating agent (e.g. methyllithium) and as necessary, an OH-protecting group is removed. Thereby, a compound of formula IV is preferably obtained.

    METHOD FOR SYNTHESIZING HYDRAZINIUM NITROFORMATE

    公开(公告)号:JPH07291901A

    公开(公告)日:1995-11-07

    申请号:JP10893494

    申请日:1994-04-25

    Abstract: PURPOSE:To provide a method for synthesizing hydrazinium nitroformate, capa ble of securing the safety, simply synthesizing the objective compound and raising the yield, by maintaining optimum reaction conditions and establishing safe handling of an intermediate. CONSTITUTION:In synthesizing hydrazinium nitroformate (HNF) by using acetic anhydride and nitric acid, (1) acetic anhydride 18 reacted with fuming nitric acid (1.52 specific gravity) at 25 to 30 deg.C while successively continuing stirring to synthesize tetranitromethane. (2) The tetranitromethane is reacted with potassium.hydroxide in an aqueous solution of glycerol to provide a potassium salt of trinitromethane (nitroform as another name) and then (3) the potassium salt is reacted with sulfuric acid prepared by diluting concentrated sulfuric acid with water (about 1:1). Nitroform dissolved in water together with nitroform made into an oily state and floating on the upper layer is extracted with an ether while cooling with water and the ether recovered to provide the nitroform. (4) The prepared nitroform is dissolved in methanol and reacted with hydrazine hydrate to provide HNF.

    SYNTHESIS OF 3-(5-NITROCYCLOHEX-1-ENYL) ACRYLIC ACID AND ESTERS THEREOF
    298.
    发明申请
    SYNTHESIS OF 3-(5-NITROCYCLOHEX-1-ENYL) ACRYLIC ACID AND ESTERS THEREOF 审中-公开
    3-(5-硝基环己-1-烯基)丙烯酸及其酯的合成

    公开(公告)号:WO2008005344A3

    公开(公告)日:2008-04-03

    申请号:PCT/US2007015152

    申请日:2007-06-29

    Abstract: This application discloses provides a process for the introduction of nitro-group functionality into a compound which contains also a site of unsaturation and/or oxygen functionality by direct (one step) oxidation of an oxime functional group mediated by a molybdenum VI/VII peroxo complex, the process comprising: (a) providing a substrate of Formula I containing an oxime functional group; Chemical formula should be inserted here as it appears on the abstract in paper form. wherein R 1 and R 2 are selected independently from linear, branched or cyclic alkyl and linear, branched or cyclic alkenyl groups, optionally substituted, with the proviso that at least one of R 1 or R 2 contains a carbon/carbon double bond; and (b) contacting said substrate of Formula I with a molybdenum oxidation complex, thereby oxidizing said oxime functional group to a nitro functional group to yield the structure of Formula III. Chemical formula should be inserted here as it appears on the abstract in paper form. Where R 1 and R 2 are as defined above.

    Abstract translation: 该申请公开了提供一种通过直接(一步)氧化由钼VI / VII过氧络合物介导的肟官能团将硝基官能团引入到还含有不饱和度和/或氧官能度位点的化合物中的方法 该方法包括:(a)提供含有肟官能团的式I的底物; 化学式应插入此处,因为它以摘要形式出现在纸上。 其中R 1和R 2独立地选自任选取代的直链,支链或环状烷基和直链,支链或环状烯基,条件是至少一个 R 1或R 2含有碳/碳双键; 和(b)使所述式I的底物与钼氧化络合物接触,由此将所述肟官能团氧化成硝基官能团以产生式III的结构。 化学式应插入此处,因为它以摘要形式出现在纸上。 其中R 1和R 2如上所定义。

    PROCESS FOR THE PREPARATION OF NITRO COMPOUNDS AND METHOD FOR THE REMOVAL OF NITROGEN DIOXIDE
    299.
    发明申请
    PROCESS FOR THE PREPARATION OF NITRO COMPOUNDS AND METHOD FOR THE REMOVAL OF NITROGEN DIOXIDE 审中-公开
    硝基化合物的制备方法和去除二氧化钛的方法

    公开(公告)号:WO00069803A1

    公开(公告)日:2000-11-23

    申请号:PCT/JP2000/003112

    申请日:2000-05-16

    Abstract: A process for the preparation of nitro compounds by reacting an organic substrate with nitrogen dioxide either in the presence of oxygen or under such conditions that the nitrogen dioxide/organic substrate ratio is less than 1 by mole. The reaction may be conducted in the presence of an imide compound such as N-hydroxyphthalimide and the organic substrate includes (a) aliphatic hydrocarbons, (b) alicyclic hydrocarbons, (c) nonaromatic heterocyclic compounds having ring-constituent carbon atoms bonded to hydrogen atoms, (d) compounds bearing aromatic rings and carbon-hydrogen bonds adjacent to the rings, (e) carbonyl compounds bearing carbon-hydrogen bonds adjacent to the carbonyl groups, and so on. This process enables efficient nitration of organic substrates even under relatively mild conditions.

    Abstract translation: 通过在氧气存在下或在二氧化氮/有机底物比小于1摩尔的条件下使有机底物与二氧化氮反应来制备硝基化合物的方法。 反应可以在N-羟基邻苯二甲酰亚胺等酰亚胺化合物的存在下进行,有机基质包括(a)脂肪族烃,(b)脂环族烃,(c)具有与氢原子键合的环状结构碳原子的非芳香族杂环化合物 ,(d)带有芳环的化合物和邻近环的碳 - 氢键,(e)与羰基相邻的具有碳 - 氢键的羰基化合物等。 该方法即使在相对温和的条件下也能有效地硝化有机底物。

    ニトロベンゼン化合物を製造する方法
    300.
    发明申请
    ニトロベンゼン化合物を製造する方法 审中-公开
    制备硝基苯化合物的方法

    公开(公告)号:WO2014208296A1

    公开(公告)日:2014-12-31

    申请号:PCT/JP2014/064780

    申请日:2014-06-03

    CPC classification number: C07C201/10 C07C205/58 C07C205/12

    Abstract:  本発明の目的は、経済的に好ましくかつ工業化に適した、下記一般式(1)のニトロベンゼン化合物の製造方法を提供することにある。 一般式(1): (式中、R 1 はハロゲン原子を示し;R 2 、R 3 及びR 4 は水素原子等を示し;R 5 はハロゲン原子又はアルコキシカルボニル基を示す。) のニトロベンゼン化合物の製造方法であって、以下の工程: (i) 一般式(2):(式中、R 1 、R 2 、R 3 、R 4 及びR 5 は前記で定義した通りである。) のアニリン化合物を亜硝酸の金属塩と酸の存在下で反応させる工程; (ii) 工程(i)の生成物を亜硝酸の金属塩と銅化合物の存在下で反応させる工程、 及び工程(ii)で使用される水の総量が一般式(2)の化合物1モルに対して1.2~2.2L(リットル)であることを含む方法。

    Abstract translation: 本发明的目的是提供一种经济上有利的工业化合适的通式(1)硝基苯化合物的制备方法。 制备通式(1)的硝基苯化合物的方法(式中,R1表示卤素原子,R2,R3,R4表示氢原子等,R5表示卤素原子或烷氧基羰基) 包括以下方法:(i)使通式(2)的苯胺化合物:(在式中,R 1,R 2,R 3,R 4和R 5如前所定义)在亚硝酸金属盐存在下反应 酸和酸,和(ii)在亚硝酸金属盐和铜化合物的存在下使方法(i)的产物反应的方法; 并且相对于1摩尔通式(2)的化合物,方法(ii)中使用的水的总量为1.2-2.2L(升)。

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