Ethyl acetate nitrite

The physical piopeities of ethyl chloiide aie hsted in Table 1. At 0°C, 100 g ethyl chloride dissolve 0.07 g water and 100 g water dissolve 0.447 g ethyl chloride. The solubihty of water in ethyl chloride increases sharply with temperature to 0.36 g/100 g at 50°C. Ethyl chloride dissolves many organic substances, such as fats, oils, resins, and waxes, and it is also a solvent for sulfur and phosphoms. It is miscible with methyl and ethyl alcohols, diethyl ether, ethyl acetate, methylene chloride, chloroform, carbon tetrachloride, and benzene. Butane, ethyl nitrite, and 2-methylbutane each have been reported to form a binary azeotrope with ethyl chloride, but the accuracy of this data is uncertain (1). 

Grouping Acetone Ethane Ethyl-acetate Acetylene Ethyl amine Ethylene Acetaldehyde Ethyl glycol Crude oil Ethyl-ether Carbon disulphide Ethyl Nitrite... 

This nitrite (5 g) is dissolved in 200 ml of toluene and photolyzed For 2 hr at 20° as described above. Without further treatment the solution is chromatographed on 100 g of alumina and eluted with methylene dichloride containing increasing proportions of methanol. The first fraction gives 0.6g prednisolone BMD. The latter fractions afford 17,20 20,21-bismethylenedioxy-llj5-hydroxy-18-oximinopregna-l,4-dien-3-one (3 g) mp 270-274° [oc]d 0°, after crystallization from ethyl acetate-hexane. 

Replacement of silver nitrite by inexpensive sodiiunor potassium nitrite enhances the imlity of this process Treatment of alkenes v/ith sodiiun nitrite and iodine in ethyl acetate and water in the presence of ethylene glycol gives conjngatednitroalkenesin49-82% yield The method for generation of nitryl iodide is improved by the treatment of iodme v/ith potassium nitrite complexed v/ith 18-crovm-6 in THF under sonicadon, as shovmin Eq 2 32 ... 

Caryophyllene nitrosochloride, (CjgHgJjN OoCL, is obtained when a mixture of the sesquiterpene, alcohol, ethyl acetate, and ethyl nitrite is cooled in a freezing mixture, and then treated with a saturated solution of hydrochloric acid in alcohol. The reaction mass is allowed to stand on ice for an hour and is then exposed to sunlight. Thus prepared it melts at about 158° to 163°, and can be separated into two compounds, one being that of a-caryophyllene and the other that of yS-caryophyllene Deussen s sesquiterpenes of natural caryophyllene from clove oil), a-caryophyllene nitrosochloride melts at 177", and /3-caryophyllene nitrosochloride at 159°. They can be separated by fractional crystallisation. The corresponding a-nitrolbenzylamine melts at 126° to 128°, and the /3-nitrolbenzylamine at 172° to 173°. The bimolecular formula given above is probable but not certain. 

Nitronium tetrafluoroborate. Acetonitrile, Ammonium carbonate. Potassium carbonate. Diethyl ether, Acetone, Ethyl acetate. Butanol Sulfamic acid, Potassium hydroxide. Ethanol, Nitric acid, Sulfuric acid, Acetone, Isopropyl alcohol Dioxane, Potassium nitrite. Potassium bicarbonate, Tetranitromethane Lead acetate, Sodium azide Sodium azide, Lead acetate. Water... 

Potassium nitrate, Sulfuric acid, 1,3,5-Trifluorobenzene, Methylene chloride, Hexane, Tert-butylamine, Trifluoroacetic acid, 1,2-Dichloroethane, 3-Amino-1,2,4-traizole, Glacial acetic acid, Sodium nitrite, Urea, Ethyl acetate, Dimethylformamide, Diethyl ether, Sodium sulfate, Methanol Ethanolamine, Diethyl ether, Ethyl chlorocarbonate, Sodium hydroxide, Magnesium sulfate, Nitric acid, Anhydrous ammonia... 

Anhydrous hydrazine, Cyanogen bromide, Isopropyl alcohol, Sodium nitrite, Sodium bicarbonate, Copper nitrate cryohydrate Sodium nitrate, Sodium chloride. Sugar, Charcoal powder Potassium nitrate. Sodium chlorate. Sugar, Charcoal powder Potassium nitrate. Potassium chlorate. Sugar, Charcoal powder Sodium nitrate. Potassium chlorate. Sugar, Charcoal powder 3-Pyridol, Ethylmethylamine, Formaldehyde, Pyridine, Dimethylcarbamoyl chloride. Sodium carbonate. Chloroform, Sodium sulfate, 1,10-Dibromodecane, Acetone, Acetonitrile, Charcoal, Ethyl acetate... 

A solution of sodium nitrite (3.28 g, 48 mmol) in water (20 ml) was added to a solution of the preceding amine hydrochloride (10.0 g, 48 mmol), in concentrated HCI (40 ml), at such a rate that the temperature did not exceed -10°C. After addition was complete the solution was stirred at 0°C for 0.25 h and then added portionwise to a rapidly stirred solution of SnCI2 x 2H20 (40 g) in concentrated HCI (40 ml). The solution was warmed to room temperature and basified with 20% aqueous NaOH solution. The solution was extracted with ethyl acetate (3 x 250 ml) and the combined extracts dried (MgS04) and filtered. The solution was evaporated to dryness to give the desired hydrazine (5.0 g, 56%) m.p. 109°-112°C. 

In 2 N hydrochloric acid (0.5 ml) was dissolved 2-(4-amino-3-carboxymethylphenyl)propionic acid disodium salt, 53 mg, 0.2 mmol). Sodium nitrite (14 mg, 0.2 mmol) was added to the resulting solution under stirring and chilling with ice. The mixture was stirred for 30 minutes under chilling with ice. The mixture was then neutralized with a chilled aqueous saturated sodium acetate solution. To the neutralized mixture was added a solution of thiophenol (0.02 ml, 0.2 mmol) in 6 N aqueous sodium hydroxide solution (0.1 ml), and the mixture was stirred for 2 hours at room temperature. The reaction mixture was then made acidic by addition of 2 N hydrochloric acid, and extracted with ethyl acetate. The ethyl acetate portion was extracted with an aqueous saturated sodium hydrogen carbonate solution. The aqueous portion was then made acidic by addition of 6 N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate portion was washed successively with water and an aqueous saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 28 mg (yield 45%) of the 2-(3-carboxymethyl-4-phenylthiophenyl)propionic acid. 

Any oxidisable substrate, such as ethanol, methanol, glacial acetic acid, acetic anhydride, benzaldehyde, carbon disulfide, glycerol, glycerol, ethylene glycol, ethyl acetate, methyl acetate, and furfural Chlorates, perchlorates, permanganates Metal nitrates, nitrites, oxidants Perchlorate salts... 

A mixture of 50 g. (0.30 mole) of carbazole and 400 ml. of glacial acetic acid is heated to boiling and then cooled somewhat. Twenty-one grams (0.33 mole) of sodium nitrite is added to the stirred mixture in small portions at such a rate that the temperature of the mixture remains below the boiling point. There is next added, in the same manner as before, 83 ml. of a mixture of equal portions of acetic acid and nitric acid (sp. gr. 1.4). The precipitated crystalline material is filtered off and washed with ethanol. This material is 3-nitro-9-nitrosocarbazole, and it may be further purified by recrystallization from ethanol or ethyl acetate. 

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