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    Nitration of aromatic compounds
    23.
    发明专利
    Nitration of aromatic compounds 未知

    公开(公告)号：GB2322857A

    公开(公告)日：1998-09-09

    申请号：GB9811567

    申请日：1996-12-09

    Applicant: SECR DEFENCE

    Inventor： MILLAR ROSS WOOD ,  CLARIDGE ROBERT PETER ,  SANDALL JOHN PAUL BENET ,  THOMPSON CLAIRE

    IPC: C07C201/10 ,  C07C205/12 ,  C07C381/10 ,  C07D213/61 ,  C07D213/76 ,  C07D239/42 ,  C07D241/16 ,  C07D241/20 ,  C07D251/44 ,  C07D251/46 ,  C07B43/02 ,  C07D239/30 ,  C07D251/26 ,  C07D251/42 ,  C07D251/52

    Abstract: A method of nitrating electron-deficient carbocyclic or heterocyclic aromatic compounds such as pyridines, diazines and triazines and benzenoid aromatics having electron-withdrawing substituents involves first reacting the aromatic species with a sulphilimine species or with the corresponding N-alkali metal salt thereof to generate an N-(hetero)aryl-S,S-dialkyl, diaryl or alkylarysulphilimine derivative. This intermediate may then be readily oxidised under relatively mild conditions using a peroxycarboxylic acid such as m-chloroperbenzoic acid, peracetic or peroxytrifluoroacetic acid. Good yields of nitrated products are obtained including some previously unprepared. The novel N-alkali(alkylaryl)sulphilimine reagents are prepared by reacting an alkali metal hydride, an alkali metal hydrogenous base or an alkyl lithium with the corresponding sulphilimine. Preferred salts are the N-lithio types and the preferred sulphilimine is diphenylsulphilimine. Where the salt is used reaction should be in an aprotic solvent but if the sulphilimine per se is the reagent a polar solvent is used.

    NITRATION OF AROMATIC COMPOUNDS
    24.
    发明专利
    NITRATION OF AROMATIC COMPOUNDS 未知

    公开(公告)号：CA2240644A1

    公开(公告)日：1997-06-26

    申请号：CA2240644

    申请日：1996-12-09

    Applicant: SECR DEFENCE BRIT

    Inventor： SANDALL JOHN PAUL BENET ,  MILLAR ROSS WOOD ,  THOMPSON CLAIRE ,  CLARIDGE ROBERT PETER

    IPC: C07C201/10 ,  C07C205/12 ,  C07C381/10 ,  C07D213/61 ,  C07D213/76 ,  C07D239/42 ,  C07D241/16 ,  C07D241/20 ,  C07D251/44 ,  C07D251/46 ,  C07D251/52 ,  C07D237/12 ,  C07D239/30 ,  C07D251/42

    Abstract: A method of nitrating electron-deficient carbocyclic or heterocyclic aromatic compounds such as pyridines, diazines and triazines and benzenoid aromatics having electron-withdrawing substituents involves first reacting the aromatic species with a sulphilimine species or with the corresponding N-alkali metal salt thereof to generate an N-(hetero)aryl-S,S-dialkyl, diaryl or alkylarylsulphilimine derivative. This intermediate may then be readily oxidised under relatively mild conditions using a peroxycarboxylic acid such as m-chloroperbenzoic acid, peracetic or peroxytrifluoroacetic acid. Good yields of nitrated products are obtained including some previously unprepared. The novel N-alkali(alkylaryl)sulphilimine reagents are prepared by reacting an alkali metal hydride, an alkali metal hydrogenous base or an alkyl lithium with the corresponding sulphilimine. Preferred salts are the N-lithio types and the preferred sulphilimine is diphenylsulphilimine. Where the salt is used reaction should be in an aprotic solvent but if the sulphilimine per se is the reagent a polar solvent is used.

    25.
    发明专利
    未知

    公开(公告)号：DE68921340D1

    公开(公告)日：1995-03-30

    申请号：DE68921340

    申请日：1989-07-14

    Applicant: SECR DEFENCE BRIT

    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.

    PREPARATION OF EPOXY NITRATES
    26.
    发明专利
    PREPARATION OF EPOXY NITRATES 未知

    公开(公告)号：GB2239018A

    公开(公告)日：1991-06-19

    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

    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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