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    Process for production of 1-oxo-2-nitratocycloalkanes
    363.
    发明授权
    Process for production of 1-oxo-2-nitratocycloalkanes 失效
    1-氧代-2-硝基杂环烷烃的制备方法

    公开(公告)号：US3095442A

    公开(公告)日：1963-06-25

    申请号：US15265761

    申请日：1961-11-15

    Applicant: DU PONT

    Inventor： JOHN ARTHUR WILFRED

    IPC: C07C201/02 ,  C07C203/08

    CPC classification number: C07C203/08

    Abstract: The invention comprises 1-oxo-2-nitrato-cycloalkanes, e.g., 1-oxo-2-nitratocyclohexane, which may be made by reacting a cycloalkene with nitrogen dioxide in a liquid saturated hydrocarbon reaction medium at a temperature of -15 DEG to +25 DEG C. The product is usually immiscible with the hydrocarbon reaction medium and is allowed to form a lower layer which is separated by decantation. The nitrogen dioxide may be added directly to a solution of the cycloalkene, or a solution of the cycloalkene in a hydrocarbon may be added to a solution of nitrogen dioxide in the same solvent. Preferably a solution containing 45% by volume of the cycloalkene in the hydrocarbon solvent is added to a cooled and stirred solution of 3 volumes of liquid nitrogen dioxide in 4 volumes of the solvent and a stream of air or oxygen-containing gas is bubbled through the mixture. The cycloalkenes include cyclopentene, cyclohexene, cycloheptene, methyl cyclopentenes methyl cyclohexene or methyl cycloheptene and other alkyl derivatives in which each ring contains one, two or three substituents each having 1-20 carbon atoms. Specification 974,152 is referred to.

    Abstract translation: 本发明包括1-氧代-2-硝基 - 环烷烃，例如1-氧代-2-硝基环己烷，其可以通过使环烯烃与二氧化氮在液体饱和烃反应介质中在-15℃至+ 25℃。产物通常与烃反应介质不混溶，并允许形成通过倾析分离的下层。 二氧化氮可以直接加入到环烯烃的溶液中，或者将环烯烃在烃中的溶液加入到二氧化氮在相同溶剂中的溶液中。 优选将含有45体积％的环烯烃在烃溶剂中的溶液加入到3体积的液体二氧化氮在4体积的溶剂中的冷却和搅拌的溶液中，并将空气或含氧气体流鼓泡通过 混合物。 环烯烃包括环戊烯，环己烯，环庚烯，甲基环戊烯甲基环己烯或甲基环庚烯和其中每个环含有一个，两个或三个各自具有1-20个碳原子的取代基的其它烷基衍生物。 参考规格974,152。

    Manufacture of an alkyl nitrate
    365.
    发明授权
    Manufacture of an alkyl nitrate 失效
    制备硝酸烷基酯

    公开(公告)号：US2647914A

    公开(公告)日：1953-08-04

    申请号：US23127251

    申请日：1951-06-12

    Applicant: ICI LTD

    Inventor： ALLAN WILLIAM G ,  TOBIN THOMAS J

    IPC: C07C201/02

    CPC classification number: C07C203/04 ,  C07C201/02

    Abstract: A process for the continuous production of isopropyl nitrate by the continuous distillation of a mixture of easily volatile products from a boiling reaction mixture formed from nitric acid and isopropyl alcohol and into which separate streams of nitric acid and isopropyl alcohol are introduced and in which a urea concentration effective to destroy nitrous acid is maintained is characterized in that there is passed through said boiling reaction mixture undergoing continuous distillation a stream of gas chemically indifferent to it. The indifferent gas may be, e.g., air, nitrogen, carbon dioxide or steam. The isopropyl alcohol and also the nitric acid introduced into the reaction mixture may contain urea. In an example aqueous isopropyl alcohol and nitric acid, both containing urea, are fed into a reactor containing heated aqueous nitric acid also containing urea whilst air is passed through the reaction mixture. Crude isopropyl nitrate is continuously separated from the aqueous distillate. Isopropyl alcohol may be recovered from the aqueous layer of the condensate by fractional distillation after neutralizing the nitric acid present. Specification 379,312 is referred to.

    Manufacture of esters
    368.
    发明授权
    Manufacture of esters 失效

    公开(公告)号：US1967551A

    公开(公告)日：1934-07-24

    申请号：US61352832

    申请日：1932-05-25

    Applicant: ICI LTD

    Inventor： FERRIER CRAWFORD FREDERICK ALE

    IPC: C07C201/02

    CPC classification number: C07C201/02 ,  C07C203/04

    Abstract: In apparatus for the production of esters, the liquor circulates upwards through the tubes 2 of a still 1 and downwards through an external limb 7 which is connected with the still by pipes 5, 6. The liquid level is indicated at 10. Volatile reactants are introduced into the limb 7; any non-volatile reactant may be introduced into the still. ALSO: In the continuous production of esters, particularly of alkyl nitrates, in the liquid phase, the reaction mixture is circulated upwards through a still and downwards through an external limb connected thereto, the volatile reactants being introduced into the external stream of liquor. Non-volatile reactants may be added to the still. In the apparatus shown, the liquor circulates upwards through the tubes 2 of a still 1, and downward through the limb 7 which is connected with the still by pipes 5, 6. The liquid level is indicated at 10. For the production of ethyl nitrate a mixture of alcohol with 33 per cent nitric acid containing an excess of urea is heated in the still, and p equivalent quantities of 70 per cent nitric acid and alcohol containing a little urea are separately introduced into the limb 7. A mixture of ethyl and methyl nitrates may be made similarly from the mixed alcohols. Bye-products are removed by a branch pipe 8.

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