2-(2-butoxyethoxy)ethanol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution containing 2.00 g Food Black 2 (C.I. Food Black 2), 0.08 g LM pectin (Product Name: LM-104AS, The Copenhagen Pectin Factory Ltd.), 5.00 g of glycerol, 5.00 g of diethylene glycol, 8.00 g diethylene glycol mono-n-butyl ether, 0.80 g of Surfynol 465, and 79.12 g of ultrapure water was prepared. The solution was stirred for 2 hours and then filtered through a 5 μm stainless steel mesh. filtered through a 5 μm stainless steel mesh

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution containing 2.50 g Kayacryl Rhodamine FB (Product Name, Nippon Kayaku, C.I. Acid Red 52), 0.06 g LM pectin (Product Name: LM-104AS, The Copenhagen Pectin Factory Ltd.), 5.00 g of glycerol, 5.00 g of diethylene glycol, 8.00 g diethylene glycol mono-n-butyl ether, 0.80 g of Surfynol 465, and 78.64 g of ultrapure water was prepared. The solution was stirred for 2 hours and then filtered through a 5 μm stainless steel mesh. filtered through a 5 μm stainless steel mesh

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 24.3 G. (150 mmoles) of 2-(2-n-butoxyethoxy)ethanol is added dropwise with stirring to 250 ml. (290 mmoles) of a 12.5% phosgene solution in benzene, cooled in an ice bath and protected from moisture. The addition is carried out over a period of approximately 1 1/2 hours and stirring is continued in an ice bath for 2 hours. The solution is allowed to warm to room temperature and stirred overnight. Nitrogen is passed through the solution for several hours to remove excess phosgene and excess HCl. The solvent is removed in vacuo affording 32.9 g. of a colorless oil. The infrared spectrum revealed a strong carbonyl absorption and no hydroxy absorption. The oil is used without any further purification in the next step. The addition stirring is continued in an ice bath for 2 hours stirred overnight Nitrogen is passed through the solution for several hours to remove excess phosgene and excess HCl The solvent is removed in vacuo affording 32.9 g a strong carbonyl absorption no hydroxy absorption The oil is used without any further purification in the next step

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(2-butoxyethoxy)ethanol (1.46 g, 9 mmol) and sodium hydride (310 mg, g mmol) in dry tetrahydrofuran was added a solution of 3-(4-chloro-1,2,5-thiadiazol-3-yl)pyridine (590 mg, 3 mmol) in dry tetrahydrofuran. The reaction mixture was stirred at room temperature for 1 h. Water was added and the mixture was extracted with ether. The ether phase was dried and evaporated to give the title compound. the mixture was extracted with ether The ether phase was dried evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(2-butoxyethoxy)ethanol (1.46 g, 9 mmol) and sodium hydride (310 mg, g mmol) in dry tetrahydrofuran was added a solution of 3-(4-chloro-1,2,5-thiadiazol-3-yl)pyridine (590 mg, 3 mmol) in dry tetrahydrofuran. The reaction mixture was stirred at room temperature for 1 h. Water was added and the mixture was extracted with ether. The ether phase was dried and evaporated to give the title compound. the mixture was extracted with ether The ether phase was dried evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(2-butoxyethoxy)ethanol (1.46 g, 9 mmol) and sodium hydride (310 mg, 9 mmol) in dry tetrahydrofuran was added a solution of 3-(4-chloro-1,2,5-thiadiazol-3-yl)pyridine (590 mg, 3 mmol) in dry tetrahydrofuran. The reaction mixture was stirred at room temperature for 1 h. Water was added and the mixture was extracted with ether. The ether phase was dried and evaporated to give the title compound. the mixture was extracted with ether The ether phase was dried evaporated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(2-butoxyethoxy)ethanol (1.46 g, 9 mmol) and sodium hydride (310 mg, 9 mmol) in dry tetrahydrofuran was added a solution of 3-(4-chloro-1,2,5-thiadiazol-3-yl)pyridine (590 mg, 3 mmol) in dry tetrahydrofuran. The reaction mixture was stirred at room temperature for 1 h. Water was added and the mixture was extracted with ether. The ether phase was dried and evaporated to give the title compound. the mixture was extracted with ether The ether phase was dried evaporated

反応条件: temp:92.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 2000 ml-reaction flask equipped with a rectification column and a separating tank, 83.7 g (483 mmol) of 4-tert-butylphenylacetonitrile, 80.0 g (439 mmol) of 1,3,4-trimethylpyrazol-5-carboxylic acid ethyl ester, 640 g of heptane, and 160 g of diethylene glycol monobutyl ether were added, the atmosphere was substituted with nitrogen, then azeotropic dehydration was carried out by heating at 90 to 95° C. for 1 hour. The temperature was maintained, 93.2 g (482 mmol) of 28% sodium methoxide methanol solution was added dropwise over 3 hours, and the resulting mixture was further reacted for 10 hours. After cooling to 30° C. or less, 600 g of water was added to separate out heptane phase, and the resulting aqueous phase was washed with 160 g of heptane and 400 g of toluene was added, then pH was adjusted to 7 with 35% hydrochloric acid. After separating into phases, the toluene phase was washed two times with 160 g of water to obtain a toluene solution containing 116 g (yield 85.1%) of 3-oxo-2-(4-tert-butylphenyl)-3-(1,3,4-trimethylpyrazol-5-yl) propionitrile. Toluene was distilled off under a reduced pressure, then 120 g of di-n-butyl ether was added and completely dissolved therein at a temperature of 120° C. Thereafter, the solution was cooled to 20° C., the resulting crystal was further dispersed in 150 g of di-n-butylether, 200 g of n-hexane was added therein and stirred at 10° C. for 1 hour. The resulting crystal was filtered and washed with 150 g of n-hexane to obtain 92.3 g of 3-oxo-2-(4-tert-butyl phenyl)-3-(1,3,4-trimethylpyrazol-5-yl) propionitrile (melting point 178° C.). In a 2000 ml-reaction flask equipped with a rectification column The temperature was maintained the resulting mixture was further reacted for 10 hours After cooling to 30° C. or less to separate out heptane phase the resulting aqueous phase was washed with 160 g of heptane and 400 g of toluene was added After separating into phases the toluene phase was washed two times with 160 g of water to obtain a toluene solution

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2-(2-butoxyethoxy)ethanol (1.46 g, 9 mmol) and sodium hydride (310 mg, 9 mmol) in dry tetrahydrofuran was added a solution of 3-(3-chloro-1,2,5-thiadiazol-4-yl)pyridine (590 mg, 3 mmol) in dry tetrahydrofuran. The reaction mixture was stirred at room temperature for 1 h. Water was added and the mixture was extracted with ether. The ether phase was dried and evaporated to give the title compound. the mixture was extracted with ether The ether phase was dried evaporated

反応条件: temp:176.02; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A phenol-free strontium oleate/carbonate containing about 14% strontium was prepared by the following procedure. A mixture of 413 g of oleic acid, 600 g of Shellflex™ 6111 light mineral oil, 300 g of isodecyl alcohol, 40 g of butyl carbitol, and 4 g of triethylene glycol was heated to 176° F., and 1000 g of strontium hydroxide octahydrate was added. The reaction mixture was heated to 275° F. over a 2.5-hour period, while removing 550 g of water via a Dean-Stark trap with the aid of a nitrogen sparge at 2.0 SCFH. After the rate of water removal slowed, the nitrogen sparge was turned off, and carbon dioxide gas was added to the reaction via a subsurface addition tube at a rate of 450 ml/minute, and the water formed was continually removed. After 7 hours of carbon dioxide addition at 250-275° F., the carbon dioxide was turned off, the temperature of the reaction was raised to 300° F. and the remaining water was removed with the assistance of a nitrogen sparge at 2.0 SCFH. The reaction was then filtered hot with suction with the assistance of filter aid, yielding the overbased strontium oleate carbonate as a light yellow, clear mobile liquid. The product was analyzed to contain 14.25% strontium by weight. The reaction mixture was heated to 275° F. over a 2.5-hour period while removing 550 g of water via a Dean-Stark trap with the aid of a nitrogen sparge at 2.0 SCFH After the rate of water removal the nitrogen sparge carbon dioxide gas was added to the reaction via a subsurface addition tube at a rate of 450 ml/minute the water formed was continually removed After 7 hours of carbon dioxide addition at 250-275° F. the temperature of the reaction was raised to 300° F. the remaining water was removed with the assistance of a nitrogen sparge at 2.0 SCFH The reaction was then filtered hot with suction with the assistance of filter aid