Diacyloxy-alkanes from carboxylic acid - by electrolysis

    公开(公告)号:DE1950283A1

    公开(公告)日:1971-04-15

    申请号:DE1950283

    申请日:1969-10-06

    Applicant: BASF AG

    Abstract: The title cpds'. acyl gps. contain 1-2C-atoms and are sepd. by >=4C-atoms in the alkane. Acyloxy-alkane carboxylic acids, with 2H-atoms alpha to the carboxyl gp. and in which the acyl residue of the acyloxy gp. contains 1-2C-atoms and is sepd. from the carboxyl gp. by >=2C-atoms, are electrochemically condensed in a solvent mixture. The latter consists of 60-98 wt.% lower alcohols, 0-30 wt.% (cyclic) N-alkyl-substd. amides or lower alkane carboxylic acids and opt., 0.30 wt.% H2O, pref., methanol and formamide. Pref., the degree of neutralization of the carboxylic acid is kept at >10% and simultaneously, the current density is kept at >10, esp. 25-50 amp/dm2. Process gives yield of approx. 80%.

    2.
    发明专利
    未知

    公开(公告)号:CH597368A5

    公开(公告)日:1978-03-31

    申请号:CH931275

    申请日:1975-07-16

    Applicant: BASF AG

    Abstract: 1507920 Esters BASF AG 18 July 1975 [19 July 1974] 30186/75 Heading C2C [Also in Division C7] In electrochemical manufacture of an aromatic or heterocyclic ester by anodic acyloxylation of an aromatic or heterocyclic compound with an alkanoic acid, electrolysis is carried out in the presence of a conducting salt where R 1 , R 2 , and R 3 are the same or different and are H or alkyl, at least one being alkyl, and R 4 is H or C 1 -C 6 alkyl. The aromatic compound may be a benzene derivative, a naphthalene, anthracene, phenanthrene, acenaphthene, acenaphthylene, tetracene, perylene or chrysene; the heterocyclic compound may be quinoline or benzofuran; substituent groups on the aromatics may be alkyl, aryl, alkoxy, aryloxy, halogen, acyloxy, acylamino, cyano, nitro, or sulphonate; examples are given. Alkanoic acids mentioned are formic, acetic, propionic, butyric, valeric, isovaleric, and caproic; said salt may be made by reacting a suitable amine with such acid and may be trimethylammonium formate, acetate or propionate; triethyl ammonium formate, acetate or propionate, tri-n-butylammonium acetate, dimethylammonium formate, acetate or propionate, or diethylammonium acetate. The anode may be graphite, PbO 2 , Pt or Au, and the cathode graphite, Fe, steel or Pb; the electrode spacing may be 0À25-2 mm. and the C.D. 0À1- 30 A/dm. 2 ; a charge of 0À4-1À5 F/mole causes monoacyloxylation, and >2F/mole a higher degree. The electrolyte may comprise 5-60 wt. per cent aromatic or heterocyclic compound, 5-70% alkanoic acid, 1-20% of the salt and 0-50% of an inert co-solvent; everything apart from the product may be removed afterwards by distillation.

    4.
    发明专利
    未知

    公开(公告)号:DE2023080A1

    公开(公告)日:1971-12-02

    申请号:DE2023080

    申请日:1970-05-12

    Applicant: BASF AG

    Abstract: 1340095 Sebacic acid diesters BADISCHE ANILIN- & SODA-FABRIK AG 11 May 1971 [12 May 1970] 14117/71 Heading C2C [Also in Division C7] Sebacic acid diesters of C 4-12 alcohols, e.g. di- 2-ethylhexyl sebacate, are made by electrochemical condensation of the corresponding adipic acid monoesters, e.g. mono-2-ethylhexyl adipate, in methanolic solution additionally containing (a) 5 to 40% of a saturated mono- or poly-valent aliphatic ether, e.g. diethyl, di-isopropyl, diglycoldimethyl or -ethyl ether, or saturated cyclic ether or diether, e.g. tetrahydrofuran, tetrahydropyran or dioxane, and/or (b) 0À1 to 2% of an alkanoic acid having up to 4 C atoms, e.g. glacial acetic, propionic or butyric acid. The current flow may be continuous or intermittent, e.g. breaking for 2 to 60 seconds after flowing for 1 to 30 minutes. The C.D. may be 5 to 50 A/dm. 2 The acidic solution may be partially neutralized by adding sodium (bi)- carbonate or methoxide. The anode may be of Pt, Pt-Rh, Pt-Ir, Au, Au-Pt, Au plated or platinized Ti or Ta; the cathode may be of Pt, steel, Ni or Ti. The electrolytic cell may have permeable vibrating or impermeable pairs of electrodes.

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