Aluminum chloride-carbon disulfide

Aluminum chloride Carbon disulfide Warm for 10 minutes 74-91% 79... 

This reaction was first described as a new synthesis for mixed benzoins. A solution of the aryl glyoxal in the aromatic hydrocarbon is stirred at 0° for 3-20 hours with aluminum chloride. Carbon disulfide may be used as a solvent if necessary. The yields vary from 35% to 90%. The reaction has been extended to the preparation of a-hydroxy ketones of the types RCOCHOHAr and CHjCOCOHlCHjlAr by substituting r-butylglyoxal and biacetyl, respectively, for the aryl glyoxal. 

Chloro-l,4-napthohinone Acetyl chloride Carbon disulfide Aluminum chloride Silver nitrate Cyclohexene Ammonium persulfate Bromine... 

Reacts violently with water. Also forms a solid dihydrate, which reacts violently with more water to form a dear so In. Slowly hydrolyzed in NaOH solns forming Sb(OH) -. Forms solids with sulfur chloride, carbon disulfide, benzene, toluene, petr ether (resin formation), ether, ale, acetone, ethyl acetate- Glacial acetic acid gives a clear oin. S]ow y corrodes glass, copper, Lead. May be stored in aluminum vessels. 

Reagents acetyl chloride, carbon disulfide, dry aluminum chloride, concentrated hydrochloric acid, 5% sodiiun hydrogen carbonate, 2,4-di-nitrophenylhydrazine, sulfuric acid, and anhydrous calcium chloride. 

When a dilute solution of 6 phenylhexanoyl chloride in carbon disulfide was slowly added (over a period of eight days ) to a suspension of aluminum chloride in the same solvent it yielded a product A (C12H14O) in 67% yield Oxidation of A gave benzene 1 2 dicarboxyhc acid... 

From betizanilide imidochloride, dimethylaniline, and aluminum chloride in carbon disulfide. Shah and Chaubal, J. Chem. Soc. 1932, 650. 

A mixture of 13,3 grams of anhydrous aluminum chloride and 100 ml of carbon disulfide is added to 19,4 grams of 2-propionyloxybenzoic acid (prepared from the reaction of pro-pionyl chloride and 2-hydroxybenzoic acid). After an initial evolution of hydrogen chloride, the solvent is removed by distillation and the mixture is heated at 150° to 160°C for 4 hours. The cooled reaction mixture is treated with ice and hydrochloric acid and the product, 2-hydroxy-3-carboxypropiophenone, is obtained from the oily residue by distillation in vacuo,... 

Titanium (IV) iodide may be prepared by a variety of methods. High-temperature methods include reaction of titanium metal with iodine vapor,1-3 titanium carbide with iodine,4 titanium(IV) oxide with aluminum (III) iodide,5 and titanium (IV) chloride with a mixture of hydrogen and iodine. At lower temperatures, titanium (IV) iodide has been obtained by the combination of titanium and iodine in refluxing carbon tetrachloride7 and in hot benzene or carbon disulfide 8 a titanium-aluminum alloy may be used in place of titanium metal.9 It has been reported that iodine combines directly with titanium at room temperature if the metal is prepared by sodium reduction of titanium (IV) chloride and is heated to a high temperature before iodine is... 

B. 2a-Thiohomophthalimide. In a 500-ml., three-necked, round-bottomed flask equipped with a mechanical stirrer, a reflux condenser, and a dropping funnel are placed 150 ml. of carbon disulfide (Note 6) and 29.3 g. (0.22 mole) of anhydrous powdered aluminum chloride. The stirrer is started, and 17.7 g. (0.10 mole)... 

Cagniant and Cagniant have reported that succinoylation of benzo[6]thiophene under Friedel-Crafts conditions yields a separable mixture of the y-ketobutyric acids 42a and 43a in a ratio of 9 1 (combined yield 85%). Huang-Minlon reduction of 42a to the butyric acid (90%) followed by cyclization of the derived acid chloride (90%) was reported to yield 4-keto-l,2,3,4-tetrahydrodibenzothiophene (44a) (69% overall). Likewise, acylation of benzo[6]thiophene with the ester chloride of succinic acid in carbon disulfide-aluminum chloride gave a separable mixture (80%) of the 2- and 3-y-ketobutyric esters. Two alternative... 

Benzofuranyl)butanoic acid readily forms the acid chloride, and this undergoes intramolecular Friedel-Crafts acylation on treatment with tin(IV) chloride in carbon disulfide at room temperature, providing 1,2,3,4-tetra-hydro-l-dibenzofuranone (54%). " This intermediate has been converted to dibenzofuran by lithium aluminum hydride reduction and subsequent dehydrogenation, to 1-methyldibenzofuran by Grignard reaction and dehydrogenation, and to 1-dibenzofuranol by reaction with iV-bromosuccinimide and subsequent dehydrobromination with pyridine. 

Aluminum foil, Iodine powder. Carbon disulfide, 1,4,6,9-Tetrabromodiamantane, Sodium bisulfite. Hydrochloric acid. Methanol, Acetonitrile, Acetone, Sodium hydroxide. Magnesium sulfate. Potassium permanganate. Toluene Methylene chloride, 2-Bromomethanol, Trioxane, Aluminum chloride. Magnesium sulfate, Nitroform, Acetone, Sodium bicarbonate. Hexane, Silver nitrate. Acetonitrile 1,2-Dichloroethane, HexamethyldisUane, Iodine, Cyclohexane, 1,3-Dioxolane, Nitroform, Methylene chloride, Dimethylformamide, Sodium sulfate. Hydrochloric acid. Magnesium sulfate. Nitric acid. Sulfuric acid Sulfuryl chloride. Acetic anhydride. Nitric acid. Sodium bicarbonate. Sodium sulfate Nitric acid. Sulfuric acid, Malonamide Nitric acid. Sulfuric acid, Cyanoacetic acid Sulfuric acid, Acetasalicyclic acid. Potassium nitrate Nitroform, Diethyl ether, 1-Bromo-l-nitroethane, Sodium sulfuate... 

---