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    Solid nitrating agent incorporating dintrogen pentoxide
    1.
    发明专利
    Solid nitrating agent incorporating dintrogen pentoxide 未知

    公开(公告)号：GB2347409A

    公开(公告)日：2000-09-06

    申请号：GB9904706

    申请日：1999-03-03

    Applicant: SECR DEFENCE

    Inventor： MILLAR ROSS WOOD ,  CLARIDGE ROBERT PETER ,  PHILBIN SIMON PATRICK

    IPC: C07B43/02 ,  C07C201/02 ,  C07C203/04 ,  C07D295/28 ,  C01B21/20 ,  C07D305/06

    Abstract: A solid nitrating reagent comprises either a montmorillonite clay or a zeolite material incorporating an amount, preferably 10-30 wt 90, of gaseous dinitrogen pentoxide. The clay material can be type K10 and suitable zeolites include those designated ZSM-5, zeolite beta, zeolite F720 and zeolite F780 (all H form). The reagent is conveniently prepared by exposing a sample of the montmorillonite clay or zeolite material to gaseous dinitrogen pentoxide contained in a stream of ozonised oxygen at a sub-ambient temperature while agitating the clay or zeolite material. The temperature is in the range of -60 to -20{C. In use the reagent is contacted with a substance to be nitrated in an inert solvent such as hexane or a perfluorocarbon at a temperature of -20 to 15{C. Suitable substances to be nitrated include alcohols O-silyl ethers and silylamines.

    METHOD OF PREPARING HETEROALICYCLIC N-NITRO COMPOUNDS
    2.
    发明专利
    METHOD OF PREPARING HETEROALICYCLIC N-NITRO COMPOUNDS 未知

    公开(公告)号：CA2059786A1

    公开(公告)日：1999-11-03

    申请号：CA2059786

    申请日：1992-01-22

    Applicant: SECR DEFENCE BRIT

    Inventor： MILLAR ROSS WOOD

    IPC: C06B25/34 ,  C07B43/02 ,  C07D239/04 ,  C07D239/10 ,  C07D263/26 ,  C07D295/28 ,  C07F7/08

    Abstract: A method of preparing heteroalicyclic N-vitro compounds consists of the steps of reacting a heteroalicyclic N-monosilylated compound with dinitrogen pentoxide, preferably within an inert organic solvent and within the temperature range -10.degree.C to +10.degree.C, and separating the N-vitro product from the silyl nitrate co-product thus obtained. The present nitrodesilylation method is capable of producing heteroalicyclic N-vitro compounds in high yields of typically 60-80%, and generates a silyl nitrate co-product which is relatively easy to remove by distillation in the presence of excess N2O5. Reagents containing two or more N-silyl groups per molecule can be employed yielding useful high explosive materials containing a corresponding number of N-vitro groups per molecule.

    PREPARATION OF NITRATOALKYL-SUBSTITUTED CYCLIC ETHERS
    4.
    发明专利
    PREPARATION OF NITRATOALKYL-SUBSTITUTED CYCLIC ETHERS 未知

    公开(公告)号：GB2240779A

    公开(公告)日：1991-08-14

    申请号：GB9101361

    申请日：1991-01-18

    Applicant: SECR DEFENCE

    Inventor： PAUL NORMAN CHARLES ,  MILLAR ROSS WOOD ,  GOLDING PETER

    IPC: C07D303/16 ,  C07D305/06

    Abstract: PCT No. PCT/GB89/00812 Sec. 371 Date Mar. 22, 1991 Sec. 102(e) Date Mar. 22, 1991 PCT Filed Jul. 14, 1989 PCT Pub. No. WO90/01028 PCT Pub. Date Feb. 8, 1990.A continuous process for producing nitratoalkyl-substituted cyclic ethers which consists of (a) cocurrently mixing a stream of N2O5 and a stream of a hydroxyalkyl-substituted cyclic ether each dissolved in an inert organic solvent, followed by (b) rapidly separating the nitric acid and nitratoalkyl coproducts before they can react together to rupture the ether ring. Step (b) is conveniently performed by quenching the product stream within approximately 15 seconds of its formation, in a basic aqueous solution into which the nitric acid is transferred from the organic phase and is neutralized. Examples of products which may be prepared by this process are nitratoalkyl-substituted oxiranes and oxetanes.

    PREPARATION OF EPOXY NITRATES
    8.
    发明专利
    PREPARATION OF EPOXY NITRATES 未知

    公开(公告)号：GB2239018B

    公开(公告)日：1992-01-08

    申请号：GB9101362

    申请日：1991-01-18

    Applicant: SECR DEFENCE

    Inventor： MILLAR ROSS WOOD ,  PAUL NORMAN CHARLES ,  GOLDING PETER

    IPC: C07D303/16 ,  C07D305/06 ,  C07D301/00

    Abstract: PCT No. PCT/GB89/00813 Sec. 371 Date Mar. 22, 1991 Sec. 102(e) Date Mar. 22, 1991 PCT Filed Jul. 14, 1989 PCT Pub. No. WO90/01029 PCT Pub. Date Feb. 8, 1990.A method of preparing a nitrate ester of an epoxy alcohol, which consists of reacting an epoxy alcohol with N2O5 in an inert solvent at a temperature of -10 DEG C. to -40 DEG C., followed by quenching the reaction mixture in aqueous solution. Quenching separates the nitric acid and nitrate ester coproducts into aqueous and organic phases respectively to prevent subsequent reaction between the two. Reaction between the nitric acid coproduct and epoxy alcohol reagent to produce acyclic contaminants is supressed by adding the epoxy alcohol to excess N2O5, thereby rapidly converting available alcohol to nitrate ester.

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