4-羟基-4-甲基-2-戊酮

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask blanketed with nitrogen was charged with 3-isopropenyl-α,α-dimethylbenzylisocyanate (m-TMI) (475.33 g) and the isocyanate was heated to about 85° C. 4-hydroxy-4-methyl-2-pentanone (274.99 g) was added from an addition funnel to the flask at a fairly rapid rate. The mixture was stirred for two hours and about 0.16 g of dibutyltin dilaurate was added to the mixture, after which the temperature was raised to about 100° C. The reaction mixture was stirred for about 1.5 hours at 100° C. and then allowed to cool and stand at room temperature for approximately 48 hours. Subsequently, about 0.14 g of additional dibutyltin laurate was added and heating at 100° C. was resumed. The reaction mixture temperature was then raised to about 125°-130° C. and the mixture was stirred overnight. Water (800 ml) was added to the cooled reaction mixture and the mixture was distilled. The remaining material in the distillation pot was extracted with toluene. The toluene extract was dried with anhydrous K2CO3, the toluene was distilled and the title product was recovered in a toluene solution. A flask blanketed with nitrogen The reaction mixture was stirred for about 1.5 hours at 100° C. to cool stand at room temperature for approximately 48 hours heating at 100° C. The reaction mixture temperature was then raised to about 125°-130° C. the mixture was stirred overnight the mixture was distilled The remaining material in the distillation pot was extracted with toluene The toluene extract was dried with anhydrous K2CO3 the toluene was distilled the title product was recovered in a toluene solution

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4-hydroxy-4-methyl-2-pentanone (10.0 g, 85.7 mmole) and hydroxylamine hydrochloride (22.17 g, 343 mmole) in 90 ml of water was stirred vigorously at room temperature. To this solution was added slowly over a period of an hour solid sodium bicarbonate (26.8 g, 343 mmole). After 3 hours the reaction mixture was extracted with ethyl acetate (3×, 100 ml), dried (MgSO4) and evaporated under reduced pressure, to give the product as an oil. Yield 11.2 g After 3 hours the reaction mixture was extracted with ethyl acetate (3×, 100 ml) dried (MgSO4) evaporated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4-hydroxy-4-methyl-2-pentanone (10.0 g, 85.7 mmole) and hydroxylamine hydrochloride (22.17 g, 343 mmole) in 90 ml of water was stirred vigorously at room temperature. To this solution was added slowly over a period of an hour solid sodium bicarbonate (26.8 g, 343 mmole). After 3 hours the reaction mixture was extracted with ethyl acetate (3×, 100 ml), dried (MgSO4) and evaporated under reduced pressure, to give the product as an oil. Yield 11.2 g After 3 hours the reaction mixture was extracted with ethyl acetate (3×, 100 ml) dried (MgSO4) evaporated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Acetone under the reaction conditions forms also some diacetone alcohol and mesityl oxide, and these then react with the prenyl chloride to produce the above isomers of prenyl mesityl oxide, also called prenyl-substituted methyl pentenones, in the same manner as acetone reacts with prenyl chloride to produce methyl heptenone. It is also possible that prenyl chloride reacts with the diacetone alcohol in the same manner to give the corresponding hydroxy derivatives that subsequently dehydrate. The presence of such hydroxy ketones is observed in the residues of the methyl heptenone production by the process of U.S. Pat. No. 3,668,255.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Acetone under the reaction conditions forms also some diacetone alcohol and mesityl oxide, and these then react with the prenyl chloride to produce the above isomers of prenyl mesityl oxide, also called prenyl-substituted methyl pentenones, in the same manner as acetone reacts with prenyl chloride to produce methyl heptenone. It is also possible that prenyl chloride reacts with the diacetone alcohol in the same manner to give the corresponding hydroxy derivatives that subsequently dehydrate. The presence of such hydroxy ketones is observed in the residues of the methyl heptenone production by the process of U.S. Pat. No. 3,668,255.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Acetone under the reaction conditions forms also some diacetone alcohol and mesityl oxide, and these then react with the prenyl chloride to produce the above isomers of prenyl mesityl oxide, also called prenyl-substituted methyl pentenones, in the same manner as acetone reacts with prenyl chloride to produce methyl heptenone. It is also possible that prenyl chloride reacts with the diacetone alcohol in the same manner to give the corresponding hydroxy derivatives that subsequently dehydrate. The presence of such hydroxy ketones is observed in the residues of the methyl heptenone production by the process of U.S. Pat. No. 3,668,255.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Acetone under the reaction conditions forms also some diacetone alcohol and mesityl oxide, and these then react with the prenyl chloride to produce the above isomers of prenyl mesityl oxide, also called prenyl-substituted methyl pentenones, in the same manner as acetone reacts with prenyl chloride to produce methyl heptenone. It is also possible that prenyl chloride reacts with the diacetone alcohol in the same manner to give the corresponding hydroxy derivatives that subsequently dehydrate. The presence of such hydroxy ketones is observed in the residues of the methyl heptenone production by the process of U.S. Pat. No. 3,668,255.

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 22.4 g DP9C/012, 3.9 g Poly G 83-34, 1.0 g Pluronic L-62, 0.4 g trimethylolethane, 2.0 g Cirrasol G-265, 1.0 g DMAMP DBS, and 0.11 g tin catalyst are added to 2.6 g N-methyl pyrrolidone plus 4.7 g methylethylketone, 2.8 g tertiary amyl alcohol, 0.6 g 2,4-pentanedione and 4.0 g diacetone alcohol and are mixed together. The mixture is heated to 60° C. and then reacted for 6 hours in a nitrogen atmosphere. Following the reaction, the resulting polyurethane prepolymer mixture is cooled and then dispersed in 59.0 g of distilled water, 0.1 g trimethylolethane, and 0.2 g triethanolamine with a high shear disperser, resulting in a stable aqueous polyurethane dispersion having about 24% solids by weight of the dispersion. The resulting polyurethane comprises about 3% polyethylene oxide side chains by weight of the solids of the polyurethane, about 12% polyethylene oxide main chains by weight of the solids of the polyurethane, and about 48% blocked polyisocyanates by weight of the solids of the polyurethane. are mixed together reacted for 6 hours in a nitrogen atmosphere the reaction

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 40 g of ammonia gas is introduced in the course of about 4 hours at 13°-15°C into a mixture consisting of 126 g of acetone, 22.5 g of methanol and 4.7 g of ammonium chloride. The reaction mixture is subsequently stirred for a further 30 minutes at the same temperature. An addition is then made to the reaction mixture of 220 g of diacetone alcohol and 110 g of acetone; the whole is heated within 1 hour to 55°C and held at this temperature for 12 hours. Processing by fractional distillation yields 125 g of 2,2,6,6-tetramethyl-4-oxopiperidine. An addition the whole is heated within 1 hour to 55°C held at this temperature for 12 hours Processing by fractional distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 40 g of ammonia gas is introduced in the course of about 4 hours at 13°-15°C into a mixture consisting of 126 g of acetone, 22.5 g of methanol and 4.7 g of ammonium chloride. The reaction mixture is subsequently stirred for a further 30 minutes at the same temperature. An addition is then made to the reaction mixture of 220 g of diacetone alcohol and 110 g of acetone; the whole is heated within 1 hour to 55°C and held at this temperature for 12 hours. Processing by fractional distillation yields 125 g of 2,2,6,6-tetramethyl-4-oxopiperidine. An addition the whole is heated within 1 hour to 55°C held at this temperature for 12 hours Processing by fractional distillation

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask blanketed with nitrogen was charged with 3-isopropenyl-α,α-dimethylbenzylisocyanate (m-TMI) (475.33 g) and the isocyanate was heated to about 85° C. 4-hydroxy-4-methyl-2-pentanone (274.99 g) was added from an addition funnel to the flask at a fairly rapid rate. The mixture was stirred for two hours and about 0.16 g of dibutyltin dilaurate was added to the mixture, after which the temperature was raised to about 100° C. The reaction mixture was stirred for about 1.5 hours at 100° C. and then allowed to cool and stand at room temperature for approximately 48 hours. Subsequently, about 0.14 g of additional dibutyltin laurate was added and heating at 100° C. was resumed. The reaction mixture temperature was then raised to about 125°-130° C. and the mixture was stirred overnight. Water (800 ml) was added to the cooled reaction mixture and the mixture was distilled. The remaining material in the distillation pot was extracted with toluene. The toluene extract was dried with anhydrous K2CO3, the toluene was distilled and the title product was recovered in a toluene solution. A flask blanketed with nitrogen The reaction mixture was stirred for about 1.5 hours at 100° C. to cool stand at room temperature for approximately 48 hours heating at 100° C. The reaction mixture temperature was then raised to about 125°-130° C. the mixture was stirred overnight the mixture was distilled The remaining material in the distillation pot was extracted with toluene The toluene extract was dried with anhydrous K2CO3 the toluene was distilled the title product was recovered in a toluene solution