Strontium dihydroxide octahydrate

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

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

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

実験手順: A solution of 2.34 g (3 millimoles) of digoxin is treated with 797 mg (3 millimoles) of strontium hydroxide octahydrate and the mixture is methylated with 757 g (6 millimoles) of dimethyl sulfate at 0° C., the procedure being the same as in Example 6. Evaporation of the fractions collected gives 119 mg (4.90% of theory of dimethyldigoxin, 403 mg (17.16%) of digoxin and 1.732 g (72.62% of theory) of β-methyldigoxin, from which 1.59 g of pure β-methyldigoxin are obtained after recrystallization from acetone. The yield is 66.67% and the selectivity of the reaction is 80.48%. Evaporation of the fractions collected

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100 of myristic acid which has been granulated from an aqueous emulsion as described in Example 1 (AN 246, titer 53° C. particle size 0.2-0.3 mm.) and 60.2 g strontium hydroxide octahydrate (97% active) are suspended in one liter of water at 50° C. temperature and stirred for 30 minutes at 50° C. followed by 60 minutes of agitation at 70° C. The hollow formed granulate is filtered and dried. The content of free fatty acid amounts to 1.7%. titer 53° C. followed by 60 minutes of agitation at 70° C The hollow formed granulate is filtered dried

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100 of myristic acid which has been granulated from an aqueous emulsion as described in Example 1 (AN 246, titer 53° C. particle size 0.2-0.3 mm.) and 60.2 g strontium hydroxide octahydrate (97% active) are suspended in one liter of water at 50° C. temperature and stirred for 30 minutes at 50° C. followed by 60 minutes of agitation at 70° C. The hollow formed granulate is filtered and dried. The content of free fatty acid amounts to 1.7%. titer 53° C. followed by 60 minutes of agitation at 70° C The hollow formed granulate is filtered dried

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

実験手順: Strontium hydroxide octahydrate (1.0 g, 3.79 mmol) and L-alanine (0.67 g, 7.52 mmol) in water (30 ml) were stirred for 4 hours at room temperature. The mixture was filtered and the filtrate was evaporated to dryness and dried in vaccuo at ambient temperature. Yield 0.81 g (63%). The mixture was filtered the filtrate was evaporated to dryness dried in vaccuo at ambient temperature

反応条件: temp:4.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 222 g of 70% 1,3-propanedisulphonic acid in water (0.76 mol) and 200.4 g of strontium hydroxide octahydrate (0.75 mol) in 200 ml of water is heated at reflux for 3 hours. The reaction mixture is filtered hot and then cooled to 4° C. The precipitate formed is removed by filtration and 500 ml of 96% ethanol are added to the filtrate. The precipitate is filtered off, rinsed with 250 ml of a 70/30 ethanol/water mixture and dried to obtain 139 g of a white crystalline product of 1,3-propanedisulphonic acid strontium salt (yield 63%). is heated at reflux for 3 hours The reaction mixture is filtered hot The precipitate formed is removed by filtration and 500 ml of 96% ethanol are added to the filtrate The precipitate is filtered off rinsed with 250 ml of a 70/30 ethanol/water mixture dried

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 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

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

実験手順: Strontium hydroxide octahydrate (1.0 g, 3.79 mmol) and L-alanine (0.67 g, 7.52 mmol) in water (30 ml) were stirred for 4 hours at room temperature. The mixture was filtered and the filtrate was evaporated to dryness and dried in vaccuo at ambient temperature. Yield 0.81 g (63%). The mixture was filtered the filtrate was evaporated to dryness dried in vaccuo at ambient temperature

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

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

実験手順: A solution of 2.34 g (3 millimoles) of digoxin is treated with 797 mg (3 millimoles) of strontium hydroxide octahydrate and the mixture is methylated with 757 g (6 millimoles) of dimethyl sulfate at 0° C., the procedure being the same as in Example 6. Evaporation of the fractions collected gives 119 mg (4.90% of theory of dimethyldigoxin, 403 mg (17.16%) of digoxin and 1.732 g (72.62% of theory) of β-methyldigoxin, from which 1.59 g of pure β-methyldigoxin are obtained after recrystallization from acetone. The yield is 66.67% and the selectivity of the reaction is 80.48%. Evaporation of the fractions collected

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 100 of myristic acid which has been granulated from an aqueous emulsion as described in Example 1 (AN 246, titer 53° C. particle size 0.2-0.3 mm.) and 60.2 g strontium hydroxide octahydrate (97% active) are suspended in one liter of water at 50° C. temperature and stirred for 30 minutes at 50° C. followed by 60 minutes of agitation at 70° C. The hollow formed granulate is filtered and dried. The content of free fatty acid amounts to 1.7%. titer 53° C. followed by 60 minutes of agitation at 70° C The hollow formed granulate is filtered dried