公开(公告)号：GB896445A

公开(公告)日：1962-05-16

申请号：GB572560

申请日：1960-02-18

Applicant: BASF AG

Inventor： HIEBER WALTER

IPC: C01G47/00

Abstract: Rhenium pentacarbonyl hydride H.Re(CO)5 is prepared by reacting rhenium pentacarbonyl with an alkali metal amalgam, or a finely divided alkali metal in the presence of an inert solvent, or a solution of an alkali metal in liquid ammonia, to form an alkali metal pentacarbonyl rhenate which is treated with a non-oxidizing acid or acid salt. Alternatively, the solution of alkali metal pentacarbonyl rhenate prepared by the same reaction is treated with a tri-ortho-phenanthroline nickel (II) salt, or with the cation complex [Cr(C6H6)2]+ or [Co(C5H5)2]+, to precipitate a complex salt which is separated and treated with a non-oxidizing acid or acid salt to obtain the pentacarbonyl hydride. Inert solvents may be tetrahydrofuran, furfural, diethyl ether, dimethyl glycol ether, or dioxan. The reaction may be effected at 15 DEG -80 DEG C. and superatmospheric pressure. The acid may be phosphoric, and the alkali metal (Li, Na, K, Rb, and Cs are all specified) may be of size 0,1 mm. and below.

公开(公告)号：CA659678A

公开(公告)日：1963-03-19

申请号：CA659678D

Applicant: BASF AG

Inventor： HIEBER WALTER

公开(公告)号：GB883280A

公开(公告)日：1961-11-29

申请号：GB780459

申请日：1959-03-06

Applicant: BASF AG

Inventor： HIEBER WALTER ,  WAGNER GERHARD

IPC: C01G45/04

Abstract: Manganese pentacarbonyl hydride is prepared by dissolving manganese pentacarbonyl in an inert polar organic liquid, adding a free-H ion containing medium and treating the resulting solution with a reducing agent. In a modification the manganese pentacarbonyl may be dissolved in the inert polar organic liquid to which the free-H ion-containing medium has already been added. Reference is made to the use, as inert polar organic liquids, of alcohols, e.g. methyl-, ethyl- or propyl-alcohol or ethers, e.g. diethyl-, or dibutyl-ether, tetrahydrofuran, glycol ethers, dimethyl formamide or dioxane. The free-H ion containing medium may be aqueous solutions of acids, e.g. sulphuric or hydrochloric acids, or organic acids such as formic or acetic, acid salts, e.g. sodium hydrogen sulphate or sodium dihydrogen phosphate or salts which react with water to form acids, for example aluminium trichloride. The reducing agent may be any compound having a reducing action in acid solution, the use of metals, e.g. magnesium and aluminium, metal alloys and amalgams, the compound NaHSO2-CH2O, dithionite and formamidine sulphinic acid being specifically referred to. The reaction may be carried out at normal or elevated temperatures preferably between 5 DEG C. and 100 DEG C. and at normal or increased pressure. Specification 855,065 is referred to.

公开(公告)号：FR1218820A

公开(公告)日：1960-05-12

申请号：FR789158

申请日：1959-03-12

Applicant: BASF AG

Inventor： HIEBER WALTER ,  WAGNER GERHARD

IPC: C01G45/04

公开(公告)号：FR1250116A

公开(公告)日：1961-01-06

申请号：FR818492

申请日：1960-02-15

Applicant: BASF AG

Inventor： HIEBER WALTER

IPC: C01G47/00

公开(公告)号：FR1231709A

公开(公告)日：1960-10-03

申请号：FR789159

申请日：1959-03-12

Applicant: BASF AG

Inventor： HIEBER WALTER ,  WAGNER GERHARD

IPC: C01G45/04

公开(公告)号：FR1226079A

公开(公告)日：1960-07-08

申请号：FR796006

申请日：1959-05-29

Applicant: BASF AG

Inventor： HIEBER WALTER

IPC: B01J31/20 ,  C07F15/06

公开(公告)号：CA594832A

公开(公告)日：1960-03-22

申请号：CA594832D

Applicant: BASF AG

Inventor： HIEBER WALTER ,  WAGNER GERHARD

公开(公告)号：GB873153A

公开(公告)日：1961-07-19

申请号：GB1862158

申请日：1958-06-11

Applicant: BASF AG

Inventor： HIEBER WALTER

IPC: C07F9/02 ,  C07F9/66 ,  C07F9/70 ,  C07F9/90 ,  C07F17/00

Abstract: The invention comprises manganese carbonyl complexes of formula [Mn(CO)4.X.R3]n in which X is arsenic, antimony or phosphorus, R is an aryl, oxyaryl, alkyl or oxyalkyl radical and n is equal to 1 or 2. Compounds specified include triphenyl phosphine tetracarbonyl manganese, triphenyl arsine tetracarbonyl manganese, triphenyl stibine tetracarbonyl manganese, bis-(triphenyl phosphite tetracarbonyl manganese) and triethyl phosphine tetracarbonyl manganese They may be prepared by reacting manganese pentacarbonyl with a trivalent compound of arsenic, antimony or phosphorus such as the arsines, stibines and phosphines, trivalent halogen and oxygen compounds including acids, salts and esters. The reaction is preferably carried out while excluding oxygen in the presence of an indifferent solvent, e.g. benzene and other aromatic and/or aliphatic hydrocarbons, alcohols and ethers, and at a temperature of 80 DEG C. or higher.

公开(公告)号：GB858494A

公开(公告)日：1961-01-11

申请号：GB1875459

申请日：1959-06-02

Applicant: BASF AG

Inventor： HIEBER WALTER

IPC: C07F15/06

Abstract: Complex cobalt-organo compounds of the general formula: wherein X represents a cycloalkanone, aromatic ketone or cyclic di-ether, and n is the number 1 or a fraction of 1, are produced by reacting dicobalt octacarbonyl, in an inert solvent at a temperature below 50 DEG C., with the cyclo-alkanone, aromatic ketone or cyclic diether. Specified compounds which will complex with cobalt in this way are: acetophenone, benzophenone, propiophenone, benzil and cyclo-alkanones containing from 5 to 15 carbon atoms, e.g. cyclohexanone or cyclo-octanone. Suitable inert solvents for carrying out the reaction are: petroleum ether, cyclohexane, benzene, toluene, xylenes and mesitylene. The complex compounds may be isolated in a substantially pure, crystalline state. There are six examples, in all of which n is either 1/2 or 1/4 . The complex compounds may be used as catalysts in the carbonylation of unsaturated hydrocarbons or compounds containing hydroxyl groups. The organic ligand of the cation may be replaced by ammonia (see Group III).ALSO:Hexammine cobalt (II) bis-(tetracarbonyl cobaltate) is produced when ammonia is led into an acetone-petroleum ether solution of a complex cobalt-organo compound of the formula: wherein X represents benzil and n is 1/4 (see Group IV(b)).