7-chloroheptan-1-ol

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

実験手順: A mixture of 44 g of heptane diol, 400 ml of concentrated hydrochloric acid, 150 ml of toluene and 50 ml of water was stirred for two and half hours at reflux. The toluene fraction was removed and 200 ml of toluene were added to the aqueous fraction and the mixture was heated for five hours at 85° C. to 90° C. The toluene was removed and 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase. The mixture was heated for five hours, then cooled and the organic fraction was combined with the two preceding toluene fractions. The toluene fraction was washed with water, dried and evaporated to dryness under reduced pressure, then distilled at 70° C. under 0.5 mm of mercury to obtain 37 g of the desired product. at reflux The toluene fraction was removed 200 ml of toluene were added to the aqueous fraction the mixture was heated for five hours at 85° C. to 90° C The toluene was removed 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase The mixture was heated for five hours cooled The toluene fraction was washed with water dried evaporated to dryness under reduced pressure distilled at 70° C. under 0.5 mm of mercury

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

実験手順: A mixture of 44 g of heptane diol, 400 ml of concentrated hydrochloric acid, 150 ml of toluene and 50 ml of water was stirred for two and half hours at reflux. The toluene fraction was removed and 200 ml of toluene were added to the aqueous fraction and the mixture was heated for five hours at 85° C. to 90° C. The toluene was removed and 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase. The mixture was heated for five hours, then cooled and the organic fraction was combined with the two preceding toluene fractions. The toluene fraction was washed with water, dried and evaporated to dryness under reduced pressure, then distilled at 70° C. under 0.5 mm of mercury to obtain 37 g of the desired product. at reflux The toluene fraction was removed 200 ml of toluene were added to the aqueous fraction the mixture was heated for five hours at 85° C. to 90° C The toluene was removed 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase The mixture was heated for five hours cooled The toluene fraction was washed with water dried evaporated to dryness under reduced pressure distilled at 70° C. under 0.5 mm of mercury

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether

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

実験手順: A mixture of 44 g of heptane diol, 400 ml of concentrated hydrochloric acid, 150 ml of toluene and 50 ml of water was stirred for two and half hours at reflux. The toluene fraction was removed and 200 ml of toluene were added to the aqueous fraction and the mixture was heated for five hours at 85° C. to 90° C. The toluene was removed and 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase. The mixture was heated for five hours, then cooled and the organic fraction was combined with the two preceding toluene fractions. The toluene fraction was washed with water, dried and evaporated to dryness under reduced pressure, then distilled at 70° C. under 0.5 mm of mercury to obtain 37 g of the desired product. at reflux The toluene fraction was removed 200 ml of toluene were added to the aqueous fraction the mixture was heated for five hours at 85° C. to 90° C The toluene was removed 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase The mixture was heated for five hours cooled The toluene fraction was washed with water dried evaporated to dryness under reduced pressure distilled at 70° C. under 0.5 mm of mercury

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

実験手順: A mixture of 44 g of heptane diol, 400 ml of concentrated hydrochloric acid, 150 ml of toluene and 50 ml of water was stirred for two and half hours at reflux. The toluene fraction was removed and 200 ml of toluene were added to the aqueous fraction and the mixture was heated for five hours at 85° C. to 90° C. The toluene was removed and 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase. The mixture was heated for five hours, then cooled and the organic fraction was combined with the two preceding toluene fractions. The toluene fraction was washed with water, dried and evaporated to dryness under reduced pressure, then distilled at 70° C. under 0.5 mm of mercury to obtain 37 g of the desired product. at reflux The toluene fraction was removed 200 ml of toluene were added to the aqueous fraction the mixture was heated for five hours at 85° C. to 90° C The toluene was removed 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase The mixture was heated for five hours cooled The toluene fraction was washed with water dried evaporated to dryness under reduced pressure distilled at 70° C. under 0.5 mm of mercury

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

実験手順: A mixture of 44 g of heptane diol, 400 ml of concentrated hydrochloric acid, 150 ml of toluene and 50 ml of water was stirred for two and half hours at reflux. The toluene fraction was removed and 200 ml of toluene were added to the aqueous fraction and the mixture was heated for five hours at 85° C. to 90° C. The toluene was removed and 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase. The mixture was heated for five hours, then cooled and the organic fraction was combined with the two preceding toluene fractions. The toluene fraction was washed with water, dried and evaporated to dryness under reduced pressure, then distilled at 70° C. under 0.5 mm of mercury to obtain 37 g of the desired product. at reflux The toluene fraction was removed 200 ml of toluene were added to the aqueous fraction the mixture was heated for five hours at 85° C. to 90° C The toluene was removed 200 ml of toluene and 100 ml of concentrated hydrochloric acid were added to the aqueous phase The mixture was heated for five hours cooled The toluene fraction was washed with water dried evaporated to dryness under reduced pressure distilled at 70° C. under 0.5 mm of mercury

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether

反応条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g of theophylline are added under stirring at room temperature to a solution of 4.1 g of sodium hydroxide in 50 ml of water and 50 ml of methanol. After stirring the mixture at 70° C. 15.8 g of 7-chloro-1-heptanol are added. The mixture is then maintained at 70° C. for 22 hours and then it is subjected to evaporation under reduced pressure until it is dry. The residue is dissolved in 150 ml of 1-N-sodium hydroxide and the mixture is extracted with methylene chloride. After washing out with water and drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure and the oily residue is several times recrystallized from diisopropyl ether. 6.3 g of 1,3-dimethyl-7-(7'-hydroxyheptyl)-xanthine are obtained (yield, referred to reacted theophylline, =79.3%). The mixture is then maintained at 70° C. for 22 hours it is subjected to evaporation under reduced pressure until it is dry The residue is dissolved in 150 ml of 1-N-sodium hydroxide the mixture is extracted with methylene chloride After washing out with water drying over sodium sulfate the methylene chloride solution is concentrated under reduced pressure recrystallized from diisopropyl ether