Aluminum acetyl acetonate

Interestingly, salts other than tin(ll) bis-(2-ethylhexanoate) such as scandium and tin trifluoromethanesulfonate [41 3], zinc octoate [44, 45], and aluminum acetyl acetonate [45] were reported to mediate the ROP of lactones. As far as scandium trifluoromethanesulfonate is concerned, the main advantage is the increase of its Lewis acidity enabling the polymerization to be carried out at low temperatures with acceptable kinetics. Later, faster kinetics were obtained by extending the process to scandium trifluoromethanesulfonimide [Sc(NTf2)3] and scandium nonafluorobutanesulfonimide [Sc(NNf2)3] and to other rare earth metal catalysts (metal=Tm, Sm, Nd) [46]. 

Amorphous (most likely atactic) 3,4-polyisoprene of 94—100% 3,4-microstmcture was prepared with a (C2H 3A1—Ti(0—/ -C Hy) catalyst (11). Crystalline 3,4-polyisoprene containing about 70% 3,4-units and about 30% i7j -l,4-microstmcture was prepared using a catalyst derived from iron acetyl acetonate, trialkyl aluminum, and an amine in benzene (37). However, this polyisoprene contained gel and was obtained in poor yield. Essentially gel-free crystallizable 3,4-polyisoprene of 70—85% 3,4-microstmcture with the remainder being cis-1,4 microstmcture was prepared in conversions of greater than 95% with a water-modified tri alkyl aluminum, ferric acetyl acetonate, and 1,10-phenanthroline catalyst (38). The 3,4-polyisoprene is stereoregular and beheved to be syndiotactic or isotactic. 

Although formally involving the reaction with a C—H bond, metal alkoxides will react with /1-diketones and / -keto esters to form six-membered chelates and alcohols. Hence the acetyl-acetonate (acac) derivatives of aluminum can be obtained (equation 63).238... 

U the presence of the Lewis acid aluminum trichloride, acetyl-acetone (3) carries out a nucleophilic attack on chloroacetyl chlo ride (4). 

The common preparative method for 7r-allylnickel halides is at the moment the reaction of nickel(O) olefin complexes like bis(cycloocta-1,5-diene) nickel, (IV), with allylic halides (23). The olefin complex, IV, can be prepared easily by reducing nickel(II) salts (like nickel acetyl-acetonate) with aluminum organic compounds in the presence of cycloocta-1,5-diene (5). 7r-Allylnickel halides and substituted 7r-allylnickel halides prepared according to this method are listed in Table I. 

Tris. See Tris (hydroxymethyl) aminomethane Tris acetate. See Tris (hydroxymethyl) aminomethane acetate Tris (acetylacetonato) aluminum Tris (acetylacetonato) aluminum (III). See Aluminum acetylacetonate Tris (acetylacetonato) chromium (III). See Chromic acetylacetonate Tris (acetylacetonato) vanadium Tris (acetylacetonato) vanadium (III). See Vanadium tris acetyl acetonate Tris (acetylacetone) aluminum Tris (acetylacetonyl) aluminum. See Aluminum acetylacetonate... 

The interferences of aluminum, sodium fluoride, and iron(lll) have been studied [13]. The results indicate that lowering the pH is recommended. Only small amounts of Fe(lll) can be present as higher concentrations could be removed by extraction with acetyl acetone complex with CCU-... 

The polymerization of diphenyldiacetylene in the presence of vanadyl acetyl-acetonate and triethylaluminum gave an open-chain polymer 10) [13]. However, when tri(isobutyl)aluminum and titanium tetrachloride were used to catalyze polymerization of [11], the product was postulated to contain another type of repeat unit [14] 35). The soluble product from the latter polymerization possessed a cryoscopic molecular weight of 1270 and a softening point of 255°-260°C. It also had good heat resistance, losing only 3% of its weight after 6 hours at 250°C in argon. Definite catalytic activity toward the decomposition of nitrous oxide was exhibited by this product [12,14]. 

Trimethylpyrylium perchlorate has been prepared from 2,6-dimethylpyrone and methylmagnesium halides 6 from mesityl oxide and sulfoacetic acid 6 from mesityl oxide (or less satisfactorily from acetone) and a mixture of acetic anhydride and perchloric acid 7 from mesityl oxide, acetyl chloride, and aluminum chloride 8 and from <-butyl chloride, acetyl chloride,... 

Convert indole to indolyl-3-methyl-ketone (I) by treating indolyl-Mg-Br (preparation already described) with acetyl-Cl, by treating indole in POCl3 with dimethylacetamide (Vilsmeier reaction), or by reacting indole with diketene (ACS 22,1064(1968)). 15.9 g (1) in 50 ml methanol cool, stir and add dropwise 16 g Br2. Reflux 1 Vi hours on water bath cool, filter, wash with ether and recrystallize-methanol to get 18 g indolyl-3-Br-methyl-ketone (II). Dissolve 11.9 g (II) in 60 ml warm isopropanol and add 11 g 3 8% aqueous DMA (or equimoiar amount other amine) reflux one hour on water bath. Filter (recrystallize-ethanol) to get 8.5 g indolyl-3-dimethylamino-methyl ketone (III). Add 4.6 g (0.02 M) (III) in 30 ml tetrahydrofuran to 2.3 g lithium aluminum hydride in 50 ml tetrahydrofuran, stir one-half hour at room temperature and reflux two hours. Add a little water dropwise and extract the precipitate with acetone. Dry, evaporate in vacuum the combined organic phases to get an oil which will precipitate with ether-petroleum ether to give DMT. (Ill) should be tested for psychedelic activity. Dialkyltryptamines BCSJ 11,221 (1936), BSC 2291 (1966)... 

A (Alternative) JCS 3175(1952). 2 g 3-indolyl-acetic acid (preparation given elsewhere here), 1.55 g freshly fused sodium acetate, 5 ml acetic anhydride. Heat 135-140° on oil bath for eighteen hours cool, wash with water and extract with CHCl3-ether (1 4). Wash organic phase with 3X20 ml saturated KHC03 and dry, evaporate in vacuum to get the l-acetyl-3-indolyl-acetone, which can be reduced to the alpha-methyl-tryptophol derivative with lithium aluminum hydride, and then converted to the dialkyl-tryptamine as already described (as can (I)), or used in step B, or reduced to (I) as follows dissolve 1 g in 1 ml 1 N Na-methoxide in methanol and 60 ml methanol, and keep at 40° for 10 minutes acidify with dilute HC1 and extract with ether. Dry, evaporate in vacuum to get (I) (recrystallize-methanol). 

Acetylacetone has been prepared by the reaction of acetyl chloride with aluminum chloride followed by hydrolysis,3 and by the condensation of acetone with ethyl acetate under the influence of sodium,4 sodamide,5 and sodium ethoxide,5-6-7 and by the reaction of acetone and acetic anhydride in the presence of boron trifluoride.8... 

Synthesis ofLysergic Acid, By reacting N-benzoyl-3-(B-carboxyethyl)-dihydroindole (see JCS, 3158 (1931) for the preparation of this compound) with thionyl chloride, followed by aluminum chloride gives l-benzoyl-5-keto-l,2,2a,3,4,5-hexahydrobenzindole. This is then brominated to give the 4-bromo-derivative, which is converted to the ketol-ketone by reacting with methylamine acetone ethylene ketol. This is then hydrolized by acid to yield the diketone and treated with sodium methoxide to convert it to the tetracyclic ketone. Acetylate and reduce this ketone with sodium borohydride to get the alcohol, which is converted to the hydrochloride form, as usual. 

Dyong and Bendlin52 pointed out the possibility of functionalization of sorbic acid at C-3, -4, and -5 in the desired way. Introduction of two hydroxyl groups, at CA and C-5, may be accomplished stereospecifi-cally by means of cis-hvdroxylation, or by intermediation of an epoxide. Michael-type addition of a nucleophile to C-3 of the conjugated double-bond provides the possibility of obtaining all four diastereo-isomeric products. In this way, N-acetyl-DL-acosamine (137, 3-acet-amido-2,3,6-trideoxy-DL-arabmo-hexopyranose) was synthesized from 133 (obtained from the epoxide 129 in an aluminum chloride-catalyzed reaction with acetone). The amide 134 wasN-acetylated and... 

Lithium aluminum hydride reduction of pleiocarpinilam (CXLVI-D) and kopsinilam (CXLII-D) gave, respectively, N-methylkopsinyl alcohol (CXLVI-F) and kopsinyl alcohol (CXLII-F) and thus there was every likelihood that these alkaloids were the E-ring lactams derived from pleiocarpinine and kopsinine, respectively. The correctness of this view was shown by synthesis. Pleiocarpinilam was obtained by the direct permanganate oxidation of pleiocarpinine (CXLVI-A) in acetone, while kopsinilam could be prepared, in a similar manner, from N-acetyl-kopsinine (CXLIV-A) followed by acid hydrolysis of the acetyl group, or from pleiocarpine lactam A (CXLV-D) by hydrolysis and simultaneous decarboxylation of the X-carbomethoxyl followed by reesterification of the C-3 carboxylic acid. 

In a 100-mL round-bottomed flask fitted with a Hahn partial condenser, 3.36 g (0.012 mol) of 2-phthalimi-dobutyrophenone (R = CH3). 7.34 g (0.036 mol) of distilled aluminum isopropoxide and 70 mL of dry i-PrOH heated at such rate as to maintain the slow distillation of acetone. After heating the mixture for 10 h, the i-PrOH is removed in vacuo, and the residue is hydrolyzed with 10 g of tartaric acid in 50 mL of H,0 in the presence of 30 mL of benzene. The organic solution is dried and the benzene removed in vacuo crude yield 3.5 g (95.5%). The crude product is acetylated without any further purification. 

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