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    3.
    发明专利
    未知

    公开(公告)号：DE3869473D1

    公开(公告)日：1992-04-30

    申请号：DE3869473

    申请日：1988-05-27

    Applicant: HOECHST AG

    Inventor： HECK DIETER ,  HEISE HARTMUT DR ,  HINTZMANN MANFRED DR

    IPC: C07C205/38 ,  C07C67/00 ,  C07C201/00 ,  C07C201/12 ,  C07C205/31 ,  C07C205/37

    Abstract: Prodn. of 2,4-dinitrophenyl ethers of formula (I) is effected by reacting a mixt. of 1 mole 2,4-dinitrochlorobenzene (II) and 1-3 moles anhydrous alkali metal carbonate (III) in an alcohol of formula ROH (IV) at 20-150 deg.C, opt. under pressure; R1 = 1-6C alkyl or (1-4C)alkoxy(1-4C)alkyl. Pref. (III) is K2CO3. The (III):(II) molar ratio is 1.05-1.8:1. The reaction is effected at 40-120 deg.C., opt. in the presence of an inert diluent.

    PROCESS FOR THE PREPARATION OF 4-ACYLAMINO-2-ALKYLAMINOPHENYL ETHERS
    4.
    发明专利
    PROCESS FOR THE PREPARATION OF 4-ACYLAMINO-2-ALKYLAMINOPHENYL ETHERS 未知

    公开(公告)号：DE3562913D1

    公开(公告)日：1988-06-30

    申请号：DE3562913

    申请日：1985-06-13

    Applicant: HOECHST AG

    Inventor： HAHNLE REINHARD DR ,  HINTZMANN MANFRED DR ,  KOLLER WOLFGANG DR ,  PAPENFUHS THEODOR DR

    IPC: C07B61/00 ,  B01J31/00 ,  B01J31/02 ,  C07C67/00 ,  C07C231/00 ,  C07C231/02 ,  C07C231/10 ,  C07C231/12 ,  C07C233/43 ,  C07C233/75 ,  C07C301/00 ,  C07C303/34 ,  C07C303/38 ,  C07C103/44 ,  C07C102/00

    Abstract: In the prepn. of 4-acylamino-2-alkylamino -phenyl ethers of formula (I). R1 = 1-4C alkyl or 1-4C alkoxy- 1-4C alkyl or Ph opt. substd. by Cl or Br, 1-4C alkyl, 1-4C alkoxy, CF3, carboxylic acid amide, -NH-1-4C alkyl, -N(1-4C alkyl)2, -SO2-NH2, -SO2-NH-1-4C -alkyl, -SO2-N(1-4C alkyl)2, acetyl, benzoylamino or -NH-CO-1-4C-alkyl; R2 = -CO-1-4C-alkyl; R3 = 1-4C alkyl; (i) 2,4-dinitrochlorobenzene is reacted with an alkali metal alcoholate or phenolate of formula (II) R1-OM. M = alkali metal atom in a polar organic solvent, under anhydrous conditions, at -30 to +100 deg.C, to form the 2,4-dinitrophenyl ether of formula (III). (ii) After or esp. without the sepn. of the intermediate, (III) is reduced to the corresp. 2,4-diaminophenyl ether, in a polar organic solvent used in the exchange of Cl, in an H2 atmos. in the presence of a precious metal catalyst of Periodic System side-Gp. VIII (Ru to Pt), promoted by an organic N-base, at 50-120 deg.C. (iii) After or esp. without the sepn. of the intermediate, the 2,4-diaminophenyl ether is acylated selectively, in a polar organic solvent, at -30 to +90 deg.C, to the corresp. 4-acylamino-2-amino-phenyl ether of formula (IV). (iv) After or esp. without the sepn. of the intermediate, (IV) is alkylated selectively, in a polar organic solvent, with an aldehyde of formula (V) in an H2 atmos., at 30-120 deg.C, in the presence of a precious metal catalyst of Periodic System side-Gp. (VIII) (Ru to Pt), promoted by an organic N base.

    6.
    发明专利
    未知

    公开(公告)号：DE3883919D1

    公开(公告)日：1993-10-14

    申请号：DE3883919

    申请日：1988-11-04

    Applicant: HOECHST AG

    Inventor： HEISE HARTMUT DR ,  HINTZMANN MANFRED DR

    IPC: C07B61/00 ,  B01J31/02 ,  C07C67/00 ,  C07C201/00 ,  C07C201/12 ,  C07C205/19 ,  C07C205/37

    Abstract: O-Nitrophenetol is prepared by exposing 1 mol of o-nitrochlorobenzene to the action of about 1.05 to about 1.4 mol of ethanol in the presence of a phase-transfer catalyst in about 40 to about 70 per cent strength by weight alkali metal hydroxide solution at temperatures of about 50 to about 80 DEG C in such a manner that the ethanol concentration of the reaction mixture does not exceed 1.5 per cent by weight during the entire course of the reaction.

    8.
    发明专利
    未知

    公开(公告)号：DE3804621A1

    公开(公告)日：1989-08-24

    申请号：DE3804621

    申请日：1988-02-13

    Applicant: HOECHST AG

    Inventor： HEISE HARTMUT DR ,  HINTZMANN MANFRED DR

    IPC: B01J23/755 ,  C07B61/00 ,  C07C231/02 ,  C07C233/25 ,  C07C233/43

    Abstract: Process for the preparation of 4-acylamino-2-aminoalkoxybenzenes of the formula (1) … … in which R denotes a C1-C6-alkyl or C1-C4-alkoxy-C1-C4-alkylene group and R' denotes a methyl or ethyl group, by pumping a solution or suspension of a 2,4-dinitroalkoxybenzene of the formula (2) … … in which R has the said meaning, in a butyl acetate into a suspension of a nickel catalyst on a kieselguhr support in butyl acetate, which is initially introduced into an autoclave and stirred, at a hydrogen pressure of about 5 to 50 bar and a temperature of about 60 to about 120 DEG C at a rate which corresponds to the rate of hydrogenation of the 2,4-dinitroalkoxybenzene to the 2,4-diaminoalkoxybenzene, removing water from the reduction solution by azeotropic distillation after the hydrogenation and acylating the resultant 2,4-diaminoalkoxybenzene with about 0.90 to about 0.99 mol of the anhydride of an alkyl- monocarboxylic acid of 2 to 3 C atoms, relative to 1 mol of 2,4-diaminoalkoxybenzene, at about -5 to about +15 DEG C.

    10.
    发明专利
    未知

    公开(公告)号：DE58904300D1

    公开(公告)日：1993-06-17

    申请号：DE58904300

    申请日：1989-02-03

    Applicant: HOECHST AG

    Inventor： HEISE HARTMUT DR ,  HINTZMANN MANFRED DR

    IPC: B01J23/755 ,  C07B61/00 ,  C07C231/02 ,  C07C233/25 ,  C07C233/43

    Abstract: Process for the preparation of 4-acylamino-2-aminoalkoxybenzenes of the formula (1) … … in which R denotes a C1-C6-alkyl or C1-C4-alkoxy-C1-C4-alkylene group and R' denotes a methyl or ethyl group, by pumping a solution or suspension of a 2,4-dinitroalkoxybenzene of the formula (2) … … in which R has the said meaning, in a butyl acetate into a suspension of a nickel catalyst on a kieselguhr support in butyl acetate, which is initially introduced into an autoclave and stirred, at a hydrogen pressure of about 5 to 50 bar and a temperature of about 60 to about 120 DEG C at a rate which corresponds to the rate of hydrogenation of the 2,4-dinitroalkoxybenzene to the 2,4-diaminoalkoxybenzene, removing water from the reduction solution by azeotropic distillation after the hydrogenation and acylating the resultant 2,4-diaminoalkoxybenzene with about 0.90 to about 0.99 mol of the anhydride of an alkyl- monocarboxylic acid of 2 to 3 C atoms, relative to 1 mol of 2,4-diaminoalkoxybenzene, at about -5 to about +15 DEG C.

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