公开(公告)号：US3442901A

公开(公告)日：1969-05-06

申请号：US3442901D

申请日：1965-07-19

Applicant: BASF AG

Inventor： KOENIG HORST ,  METZGER HORST

IPC: C07C381/00 ,  C07C161/00 ,  C07C147/14 ,  C07D31/48

CPC classification number: C07C381/00

公开(公告)号：GB1077657A

公开(公告)日：1967-08-02

申请号：GB4556664

申请日：1964-11-09

Applicant: BASF AG

Inventor： BEER LUDWIG ,  BRUNNMUELLER FRIEDRICH ,  METZGER HORST

IPC: C07C233/09

Abstract: Contaminated solid acrylamide is purified by dissolving same in a C1- 5 aliphatic alcohol, optionally in the presence of polymerization inhibitors, separating the solution from the insoluble portion, and isolating solid acrylamide from the solution by lowering the temperature.

公开(公告)号：FR1363712A

公开(公告)日：1964-06-12

申请号：FR941876

申请日：1963-07-18

Applicant: BASF AG

Inventor： METZGER HORST ,  BEER LUDWIG

公开(公告)号：GB939149A

公开(公告)日：1963-10-09

申请号：GB239462

申请日：1962-01-23

Applicant: BASF AG

Inventor： METZGER HORST ,  WEISER DIETER

IPC: C10G11/18

Abstract: In a process for the production of ketoxime hydrochlorides by the action of nitrosating agents on aliphatic, araliphatic or cycloaliphatic hydrocarbons in the presence of actinic light, the light source is coated with an uninterrupted coherent layer of a substance in a solid form deposited by crystallisation or sublimation, this substance being the hydrocarbon reactant or an inert organic compound soluble in the reaction mixture. This coating on the light source is said to prevent the formation of a yellow-brown coloured coating upon the light source, thus preventing any decrease in the transmission of light from the source. The thickness of the crystal coating may be from 0.1 to 1.0 cm. The temperature of the reaction is maintained in the range of -30 DEG to +40 DEG C. and a temperature gradient is maintained between the light source and the reaction medium such that the crystal coating is preserved throughout the reaction. A suitable light source is an 80 watt mercury lamp providing light of wave length 200 mm to 600mm . Nitrosating agents specified are nitrosyl chloride, nitrogen monoxide and chloride, alkyl nitrites and hydrochloric acid, nitrous gases and hydrochloric acid, and nitrosylsulphuric acid and hydrochloric acid. Hydrocarbons specified as starting materials are n-hexane, n-heptane, toluene, ethylbenzene, xylenes, cyclopentane, fluorene, cyclohexane, decahydronaphthalene, cycloheptane, cyclooctane and cyclododecane; and they may be dissolved in inert solvents such as benzene, carbon tetrachloride, chloroform or monochlorobenzene. Inert organic compounds suitable for the crystal coating are naphthalene, anthracene or hexachlorethane. Four examples are given, illustrating the difference in yield and purity of ketoxime hydrochloride obtained when the reaction is carried out with and without the crystal coating on the light source. In Examples 1, 2 and 3, the crystal coatings are of cyclohexane, cyclooctane and cyclododecane respectively, and, in Example 4, a crystal coating of naphthalene is used when treating decahydronaphthalene with nitrosating agents.

公开(公告)号：CA648298A

公开(公告)日：1962-09-11

申请号：CA648298D

Applicant: BASF AG

Inventor： SCHICKH OTTO VON ,  METZGER HORST

公开(公告)号：GB871768A

公开(公告)日：1961-06-28

申请号：GB1381859

申请日：1959-04-23

Applicant: BASF AG

Inventor： SCHICKH OTTO VON ,  METZGER HORST

Abstract: The invention comprises compounds of the formula where R1, R2 and R3 represent hydrogen or an alkyl, cycloalkyl, aralkyl, aryl or acyloxy radical, an hydroxyalkyl radical etherified with alkyl or aralkyl groups or an acylated hydroxyalkyl radical, or R1 and R2 or R1 and R3 are closed by way of methylene groups or R1 and R3 are closed by way of methylene and substituted methylene groups to a cycloaliphatic ring, and n is 1 or 2; and the production of a -chloro-oximes by reacting a compound with nitrosyl chloride in the presence of hydrogen chloride and converting the a -chloro-oxime hydrochloride formed into the free a -chloro-oxime. Specified starting compounds are propylene, trimethylethylene, octene-1, octene-2, tridecene-1, cyclopentene, cyclohexene, methylcyclohexene, methylenecyclohexene, vinyl cyclohexane, limonene, cycloheptene, cyclo-octene, styrene, p-chlorostyrene, styryl acetate (PhCH:CHOCOCH3), cinnamyl acetate (PhCH:CHCH2OCOCH3), cinnamyl methyl ether and cinnamyl benzyl ether. Solvents may be used, and the process may be continuous or discontinuous.

公开(公告)号：GB846840A

公开(公告)日：1960-08-31

申请号：GB406259

申请日：1959-02-05

Applicant: BASF AG

Inventor： SCHICKH OTTO VON ,  METZGER HORST

Abstract: Cycloaliphatic ketoxime hydrochlorides are prepared by the action of nitrosyl chloride or of nitrogen monoxide and chlorine on a cycloaliphatic hydrocarbon having 5 to 10 carbon atoms in the ring in the presence of hydrogen chloride while irradiating with active light where before the reaction commences or before the reaction subsides there is added such an amount of a mixture of by-products such as are obtained as a residue from the reaction mixture arising in a reaction of cycloalkanes with a nitrosation agent of the above mentioned kind after removal of the oxime hydrochloride and the excess reactants, so that the content of organically combined chlorine in the reaction solution is at least 0,5% by weight with reference to the amount of cycloalkane used. The addition of the by-products is said to prevent the formation of a yellow coating on the lamp or glass parts of the reactor which slows down the speed of reaction. The nitrosation residues used generally contain 20 to 40% by weight of organically combined chlorine and are preferably added so that the chlorine content is 0,5 to 5% based on the hydrocarbon. The reaction is otherwise carried out in known manner and the examples describe the preparation of the oxime hydrochlorides, of cyclo-hexanone and cyclo-octanone.

公开(公告)号：GB1136116A

公开(公告)日：1968-12-11

申请号：GB1549866

申请日：1966-04-07

Applicant: BASF AG

Inventor： BECKMANN WILHELM ,  KENGELBACH WERNER LUDWIG ,  METZGER HORST ,  PAPE MARTIN

IPC: B01F15/06 ,  B01J19/12 ,  B28C7/08

Abstract: 1,136,116. Photochemical reactors. BADISCHE ANILIN-& SODA-FABRIK A.G. 7 April, 1966 [9 April, 1965], No. 15498/66. Heading B1X. A photochemical liquid phase reactor, which is especially suitable for use in the production of oximes from cycloalkanes in the presence of a solvent, has a central stirrer around which is a plurality of lamps, the diameter of a lamp being D, the inter-lamp separation is 0.3-2D, the lamp-stirrer separation is 0.05-0.5D, and the separation between the lamps and the wall is at least 0.5D. The reactor may be cylindrical with the stirrer at the axis and the lamps disposed on a circle about the axis. The stirrer may be rectangular (7 in Fig. 1, not shown), or anchor shaped (Fig. 3, not shown), and generally operates at 40-200 rpm. The cell may be cooled by elements 8, coils 10, or a cooling jacket 9 (Fig. 4, not shown). In Figs. 5 and 6 (not shown) are shown arrangements having a plurality of cells in series. In the reactor of Fig. 5, liquid flows in the direction of the arrows through cells 11 having perforate partitions 14 and stirrers 12. In the arrangement of Fig. 6, liquid flows to reactors 15, 17, 19, 21, 23, and 25 through coolers 16, 18, 20, 22, 24, and 26.

公开(公告)号：GB1120737A

公开(公告)日：1968-07-24

申请号：GB4581865

申请日：1965-10-29

Applicant: BASF AG

Inventor： KOENIG HORST ,  METZGER HORST ,  REIF WERNER

IPC: C07B61/00 ,  C07C45/00 ,  C07C45/45 ,  C07C45/67 ,  C07C45/68 ,  C07C45/72 ,  C07C49/813 ,  C07C49/84 ,  C07C205/45 ,  C07C205/51 ,  C07C317/24 ,  C07C317/44 ,  C07C323/22 ,  C07C323/52 ,  C07C323/56 ,  C07C331/02 ,  C07C331/04 ,  C07C381/00 ,  C07D213/50 ,  C08G63/12

Abstract: Compounds of formula R1-CO-CAB-R2 are prepared by reacting at 0-150 DEG C. and 1-50 atm., sulphur ylides of formula R1-CO-C( = Y)-R2 first with a solution containing an electrophile A1 and then with one containing a nucleophile B1 (or with one containing simultaneously A1 and B1). In the formulae, Y is = S(= o)Me2, = S(alkyl)2 or = SPh2, R1 is an aliphatic, araliphatic, aromatic or heterocyclic radical, an optionally substituted amino group or an ether group, and R2 is H, alkyl, aralkyl, COR1, CHR3CHR3CN or CHR3CHR3CO2 alkyl, where R3 is H or Me. The following compounds are claimed per se: R1-CO-C(O alkyl)(CHR3CHR3CN)2- with the exception of AcC(OEt)(CH2CH2CN)2- and the corresponding bis-(alkylcarboxylates), and specifically AcC(OEt)(CH2CHMeCN)2, PhNH COC(OMe)(CH2CH2CN)2 and BzC(OBu) (CHMeCH2CO2Bu)2.

公开(公告)号：GB1108062A

公开(公告)日：1968-04-03

申请号：GB3073965

申请日：1965-07-20

Applicant: BASF AG

Inventor： KOENIG HORST ,  METZGER HORST

IPC: C07C381/00 ,  C07D213/56

Abstract: A composition comprises 15 g. of styrene polymerized in 15 g pure tetrahydrofuran at 100 DEG C. under conventional conditions, with the addition of 1 g. of a compound of formula which is used as a polymerization modifier. R3 and R4 may be CH3, H, phenyl, C6H5NH-or -CH(C6H5)2. Suitable choice of R3 and R4 enables the mean M.W. of the polymer to be varied within wide limits.ALSO:Novel compounds of the formula wherein R1 and R2 are alkyl or aralkyl, R3 is H, alkyl, aralkyl, the radical or the radical where R5 is alkyl, aralkyl, or a heterocyclic 5-6 membered quasi-aromatic ring, and R4 is H, alkyl, cycloalkyl or aryl, all of which may bear up to 3 chlorine or bromine atoms as substituents, a heterocyclic 5-6 membered quasi-aromatic ring which may bear up to 3 chlorine or bromine atoms as substituents and/or is alkyl substituted and/or is annellated to a benzene nucleus, or is aralkyl, alkoxy or the radical R7R8HC-, where R7 and R8 are H or phenyl, may be prepared by reacting, if desired in the presence of a base and/or inert solvent, an oxosulphonium ylide of the formula in which R1, R2 and R3 are as defined above, with an acylating agent of formula R4R6C=O in which R4 is as defined above, and R6 is C2, Br or the radical -O-CO-R9, where R9 is defined as for R4, but is not R7R8HC-, or with an acylating agent of formula R7R8C=C=O where R7 and R8 are as defined above, at temperatures from -30 DEG C. to + 150 DEG C. Dibenzoyl methane is obtained by the reduction, using H2/Raney Ni of dimethyl-oxo-sulphurylene dibenzoyl methane. Acetoacetic anilide and acetylacetone are similarly obtained by the reduction of the requisite dimethyl - oxo - sulphurylene compounds.