Aluminum tert.-butoxide

The following preparation is given in U.S. Patent 3,356,573. 17a-Acetoxy-3(3-hydroxy-6-methylpregn-5-en-20-one (1 g), aluminum tert-butoxide (1 g) and p-benzoquinone (6 g) were dissolved in dry benzene (100 ml) and the mixture was heated under reflux for 30 minutes. The reaction mixture was cooled and washed with potassium hydroxide solution until the benzene layer was colorless. The benzene was washed with water, dried and evaporated to dryness under reduced pressure. The residue crystallized from aqueous methanol to give 17a-acetoxy-6-methylpregna-4,6-diene-3,20-dione, needles, MP 214° to 216°C. 

Acetoxolone aluminum salt Aluminum amalgam Dinoprostone Aluminum tert-butoxide Megestrol acetate Aluminum chloride Acebutolol... 

The yield is reduced by about 5 per cent by halving the amounts of acetone and benzene specified and using only 50 g. of aluminum tert.-butoxide. 

The benzene and unchanged ZerZ.-butyl alcohol are removed by distillation from the steam bath, the final traces being removed under 10-30 mm. pressure. A liter of dry ether is added, and the solid aluminum tert. -butoxide is dissolved by refluxing for a short... 

In elegant configurational studies of biphenyls, Mislow and his associates (Newman et ah, 1958 Mislow et al., 1962) have used the Meerwein-Ponndorf-Verley reduction to determine absolute configuration. Kacemic 4, l"-dinitro-l,2,3,4-dibenz-l,3-cyclohepta-diene-6-one (DNDBCH-6-one) was partially reduced (7 hours reaction time) with S-(- -)-methyl-terf-butylcarbinol and aluminum tert-butoxide to (—)DNDBCH-6-ol. The unreacted ketone was dextrorotatory. The (+)-DNDBCH-6-one was reduced to (-1-)-... 

Commercial tert.-butyl alcohol dried over calcium oxide is suitable for this preparation. Aluminum isopropoxide or ethoxide 2 may be used in place of the aluminum /er/.-butoxide to remove traces of water. The grade of metal known as fast cutting rods has proved most satisfactory. The checkers used turnings made from aluminum cast from melted-down kitchen utensils. Aluminum ferf.-butoxide has also been prepared successfully in another laboratory from commercially pure aluminum (2S) and from rods of the alloy 17ST (communication from L. F. Fieser). The checkers were able to obtain considerably higher yields of the butoxide from pure aluminum than from a copper-bearing alloy. 

Aluminum fer/.-butoxide can be prepared by refluxing dry tert. -butyl alcohol with amalgamated aluminum 5l 6 or aluminum plus mercuric chloride.6 The method described is that of Adkins and Cox.0 The preparation of amalgamated aluminum has been described.3, 4 Aluminum isopropoxide can be prepared from dry isopropyl alcohol and aluminum,1 2 the method being essentially that described for aluminum ethoxide (Org. Syn. is, 82). 

Al-containing SBA mesoporous solid was prepared as reported 9 mL tetraethyl orthosilicate (TEOS) and the calculated amount of aluminum tri-tert-butoxide, in order to obtain a well defined Si/Al ratio equal to 10, were added to 10 mL of HC1 aqueous solution at pH=1.5 water. This solution was stirred for over 3 h and then added to a second solution containing 4 g triblock poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (EO20PO70EO20 Aldrich) in 150 mL of HC1 aqueous solution at pH=1.5 at 313 K. The mixture was stirred for another 1 h and allowed to react at 373 K for 48 h. The solid product was filtered, dried at 373 K, and finally calcined in air flow (9 L h 1) at 823 K for 4 h with a heating rate of 24 K h"1. The SBA-15 was prepared according to the literature [11]. In what follows, the samples are denoted AlSBA and SBA, respectively. 

Abstract—The effects of metal alkoxide type and relative humidity on the durability of alkoxide-primed, adhesively bonded steel wedge crack specimens have been determined. Aluminum tri-sec-butoxide, aluminum tri-tert-butoxide, tetrabutyl orthosilicate, and titanium(IV) butoxide were used as alkoxide primers. Grit-blasted, acetone-rinsed mild steel adherends were the substrates bonded with epoxy and polyethersulfone. The two aluminum alkoxides significantly enhanced the durability of the adhesively bonded steel, while the titanium alkoxide showed no improvement in durability over a nonprimed control. The silicon alkoxide-primed samples gave an intermediate response. The failure plane in the adhesively bonded samples varied with the relative humidity during the priming process. 

Other experimental reproducdve effects. Human systemic effects by inhalation respirator ", nose, and eyes. Human mutation data reported. A skin and eye irritant. A sensitizer. Flammable liquid when exposed to heat or flame. Explosive reaction with aniline. Reaction with trichloroethylene forms the explosive dichloroacetylene. Ignition on contact with potassium tert-butoxide. Violent reaction with sulfuric acid or isopropylamine. Exothermic polyTTierization on contact with strong acids, caustic alkalies, aluminum, aluminum chloride, iron(III) chloride, or zinc. When heated to decomposition it emits toxic fumes of Cr. 

Carbonyl compounds act as hydrogen acceptors in the Oppenauer oxidation of alcohols to aldehydes or ketones. The reaction is based on hydride transfer from the alkoxide ion of the starting alcohol prepared in situ from anhydrous bases, aluminum isopropoxide, or, better still, tert-butoxide (equation 256). 

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