PROCESS FOR PREPARING N-SUBSTITUTED 3-HYDROXYPYRAZOLES

    公开(公告)号:CZ7498A3

    公开(公告)日:1998-09-16

    申请号:CZ7498

    申请日:1996-07-02

    Applicant: BASF AG

    Abstract: PCT No. PCT/EP96/02891 Sec. 371 Date Jan. 8, 1998 Sec. 102(e) Date Jan. 8, 1998 PCT Filed Jul. 2, 1996 PCT Pub. No. WO97/03969 PCT Pub. Date Feb. 6, 1997N-substituted 3-hydroxypyrazoles of the formula I where R1 is unsubstituted or substituted alkyl, aryl or heteroaryl and R2, R3 is hydrogen, cyano, halogen or unsubstituted or substituted alkyl, aryl or heteroaryl, are prepared by oxidation of a corresponding pyrazolidin-3-one with atmospheric oxygen in the presence of a metal salt in an essentially pH-neutral medium.

    Prepn. of trans-alkenol(s) from Wittig reaction of cyclic lactam(s) - without isolation of phosphonium salt and with isomerisation thermally or by irradiation

    公开(公告)号:DE4006919A1

    公开(公告)日:1991-09-12

    申请号:DE4006919

    申请日:1990-03-06

    Applicant: BASF AG

    Abstract: Prepn. of trans-alkenols of formula HAC=CH(CH2)nCH20H (I) comprises: (a) reaction of an alkanol of formula ACH20H (II), a term phosphine and a hydrogen halide to give a phosphonium salt of formula (III); (b) reaction of unisolated (III) with a base and a cyclic hemiacetal of formula (IV) to give a cis/trans-alkenol mix; and (c) rearrangement of the mixt. thermally or by irradiation (250-450nm) to give (I), chiefly as the trans-isomer. A = 1-16C alkyl; n = 2 or 3; R = organic gp Also claimed is a prepn. of acetate derive of (I) which comprises esterification of (I) with 0Ac0H or a derive, before or after step (c). Pref trans-dec-5-enol (Ia) and trans-tridec-4-enol (Ib). The phosphine is PPh3. Esterification takes place prior to isomerisation and the isomerisation (where esterification is carried out) is thermal. USE/ADVANTAGE - Acetylated derivs. of (Ia) and (Ib) are phenomones which may be used as pesticides. The process does not require expensive or sensitive reagents or isolation of (III) (see eg Helv Chim Actor 60, 1161 (1977)). (6pp Dwg.No.0/0)

    14.
    发明专利
    未知

    公开(公告)号:ES2195240T3

    公开(公告)日:2003-12-01

    申请号:ES98115428

    申请日:1995-10-16

    Applicant: BASF AG

    Abstract: An integrated process for the preparation of O-substituted hydroxyammonium salts of formula (I) without isolation of intermediates comprises: (a) reacting acetone with hydroxylammonium sulphate and sodium hydroxide solution to give acetone oxime of formula (II); (b) treating the obtained (II) solution with NaOH solution and completely eliminating water; (c) reacting the obtained suspension of acetone oxime sodium salt of formula (III) with an alkylating agent RY (IV) at 0.5-15 (preferably 1-4) bar and at up to 140 degrees C in presence of a phase transfer catalyst, to give an acetone oxime ether of formula (V); and (d) cleaving (V) with HX to give (I). Steps (a)-(c) are carried out in the same non-polar, aprotic solvent and step (d) is effected with concentrated acid. H2NOR.HX (I) Me2C=NOH (II) Me2C=NONa (III) Me2C=NOR (V) R = 1-6C alkyl or 2-6C alkenyl (both optionally substituted by halo); X = Cl or Br; and Y = nucleofugous group.

    15.
    发明专利
    未知

    公开(公告)号:AT234277T

    公开(公告)日:2003-03-15

    申请号:AT98115428

    申请日:1995-10-16

    Applicant: BASF AG

    Abstract: An integrated process for the preparation of O-substituted hydroxyammonium salts of formula (I) without isolation of intermediates comprises: (a) reacting acetone with hydroxylammonium sulphate and sodium hydroxide solution to give acetone oxime of formula (II); (b) treating the obtained (II) solution with NaOH solution and completely eliminating water; (c) reacting the obtained suspension of acetone oxime sodium salt of formula (III) with an alkylating agent RY (IV) at 0.5-15 (preferably 1-4) bar and at up to 140 degrees C in presence of a phase transfer catalyst, to give an acetone oxime ether of formula (V); and (d) cleaving (V) with HX to give (I). Steps (a)-(c) are carried out in the same non-polar, aprotic solvent and step (d) is effected with concentrated acid. H2NOR.HX (I) Me2C=NOH (II) Me2C=NONa (III) Me2C=NOR (V) R = 1-6C alkyl or 2-6C alkenyl (both optionally substituted by halo); X = Cl or Br; and Y = nucleofugous group.

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