propyl 3,4,5-trihydroxybenzoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Approximately 1073 grams of tertiary amine oxide such as N-methylmorpholine-N-oxide in water (76% NMMO, 24% H2O), 16 g of cellulose (DP=625, 5% moisture content) and 1.5 g stabilizer, e.g., gallic acid propyl ester, are prepared in a container and heated to above 72° C. This solution is stirred for approximately 15 minutes and about 100 g of water is then separated under vacuum. After water removal step a clear cellulose solution is obtained. Alternatively, 554 g of NMMO/water mixture (83% NMMO), 0.8 g stabilizer and 11.3 g cellulose are prepared in a container and heated to approx. 95° C. while being stirred simultaneously. After approximately 30 to 60 minutes a cellulosic solution is obtained. In this procedure it is no longer necessary to separate the water. heated to above 72° C about 100 g of water is then separated under vacuum After water removal step a clear cellulose solution is obtained while being stirred simultaneously After approximately 30 to 60 minutes a cellulosic solution is obtained to separate the water

反応条件: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Approximately 1073 grams of tertiary amine oxide such as N-methylmorpholine-N-oxide in water (76% NMMO, 24% H2O), 16 g of cellulose (DP=625, 5% moisture content) and 1.5 g stabilizer, e.g., gallic acid propyl ester, are prepared in a container and heated to above 72° C. This solution is stirred for approximately 15 minutes and about 100 g of water is then separated under vacuum. After water removal step a clear cellulose solution is obtained. Alternatively, 554 g of NMMO/water mixture (83% NMMO), 0.8 g stabilizer and 11.3 g cellulose are prepared in a container and heated to approx. 95° C. while being stirred simultaneously. After approximately 30 to 60 minutes a cellulosic solution is obtained. In this procedure it is no longer necessary to separate the water. heated to above 72° C about 100 g of water is then separated under vacuum After water removal step a clear cellulose solution is obtained while being stirred simultaneously After approximately 30 to 60 minutes a cellulosic solution is obtained to separate the water

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

実験手順: The microcrystalline cellulose, mannitol, and sucrose were screened or milled and then blended with levothyroxine sodium for about 6 minutes. Acacia, dissolved in water, and propyl gallate, dissolved in alcohol, were added over about 10 minutes to granulate the mixture. The wet granulation was dried at a temperature below 60° C. until the moisture content was less than about 4%. The dried granulation was sized by passing it through a mill, and then blended with the additional ingredients listed in the table below using conventional mixing equipment. milled were added over about 10 minutes The wet granulation was dried at a temperature below 60° C. until the moisture content

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: 1 g of chenodeoxycholic acid is dissolved in 3.4 g of sodium hydroxide solution (30 mg/ml) with warming. The solution is brought to room temperature and adjusted to pH 7.85 by addition of further sodium hydroxide solution. 500 mg of propyl gallate is then added and dissolved by shaking at room temperature. The pH is adjusted to 7.45, and 56.25 mg of recombinant human insulin is added with stirring at 37° C. After all the solid has dissolved, the solution is made up to a total weight of 8 g with distilled water, frozen and lyophilised overnight to give a dry crystalline powder. with warming is brought to room temperature dissolved is added with stirring at 37° C After all the solid has dissolved frozen to give a dry crystalline powder

反応条件: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Approximately 1073 grams of tertiary amine oxide such as N-methylmorpholine-N-oxide in water (76% NMMO, 24% H2O), 16 g of cellulose (DP=625, 5% moisture content) and 1.5 g stabilizer, e.g., gallic acid propyl ester, are prepared in a container and heated to above 72° C. This solution is stirred for approximately 15 minutes and about 100 g of water is then separated under vacuum. After water removal step a clear cellulose solution is obtained. Alternatively, 554 g of NMMO/water mixture (83% NMMO), 0.8 g stabilizer and 11.3 g cellulose are prepared in a container and heated to approx. 95° C. while being stirred simultaneously. After approximately 30 to 60 minutes a cellulosic solution is obtained. In this procedure it is no longer necessary to separate the water. heated to above 72° C about 100 g of water is then separated under vacuum After water removal step a clear cellulose solution is obtained while being stirred simultaneously After approximately 30 to 60 minutes a cellulosic solution is obtained to separate the water

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

実験手順: In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To thesolution placed in an ice bath was further added a solution of 1.94 g (10 mmol., purity 90.7%) of methyl 1-piperazinecarbodithioate in 4 ml of ethanol. The resulting mixture was then stirred for 30 min. at room temperature. To the mixture placed in an ice bath was dropwise added a solution of 2.12 g (10 mmol.) of propyl gallate in 4 ml of ethanol. The mixture was stirred overnight at room temperature and subsequently refluxed under heating for 4 hours. The mixture was cooled to room temperature. Precipitated crystals were collected by filtration and washedwith ethanol to give 1.848 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%. To thesolution placed in an ice bath To the mixture placed in an ice bath The mixture was stirred overnight at room temperature subsequently refluxed under heating for 4 hours The mixture was cooled to room temperature Precipitated crystals were collected by filtration and washedwith ethanol

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

実験手順: In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To the solution placed in an ice bath was further added a solution of 1.94 g (10 mmol., purity 90.7%) of methyl 1-piperazinecarbodithioate in 4 ml of ethanol. The resulting mixture was then stirred for 30 min. at room temperature. To the mixture placed in an ice bath was dropwise added a solution of 2.12 g (10 mmol.) of propyl gallate in 4 ml of ethanol. The mixture was stirred overnight at room temperature and subsequently refluxed under heating for 4 hours. The mixture was cooled to room temperature. Precipitated crystals were collected by filtration and washed with ethanol to give 1.843 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%. To the solution placed in an ice bath To the mixture placed in an ice bath The mixture was stirred overnight at room temperature subsequently refluxed under heating for 4 hours The mixture was cooled to room temperature Precipitated crystals were collected by filtration washed with ethanol

反応条件: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Approximately 1073 grams of tertiary amine oxide such as N-methylmorpholine-N-oxide in water (76% NMMO, 24% H2O), 16 g of cellulose (DP=625, 5% moisture content) and 1.5 g stabilizer, e.g., gallic acid propyl ester, are prepared in a container and heated to above 72° C. This solution is stirred for approximately 15 minutes and about 100 g of water is then separated under vacuum. After water removal step a clear cellulose solution is obtained. Alternatively, 554 g of NMMO/water mixture (83% NMMO), 0.8 g stabilizer and 11.3 g cellulose are prepared in a container and heated to approx. 95° C. while being stirred simultaneously. After approximately 30 to 60 minutes a cellulosic solution is obtained. In this procedure it is no longer necessary to separate the water. heated to above 72° C about 100 g of water is then separated under vacuum After water removal step a clear cellulose solution is obtained while being stirred simultaneously After approximately 30 to 60 minutes a cellulosic solution is obtained to separate the water

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

実験手順: The microcrystalline cellulose, mannitol, and sucrose were screened or milled and then blended with levothyroxine sodium for about 6 minutes. Acacia, dissolved in water, and propyl gallate, dissolved in alcohol, were added over about 10 minutes to granulate the mixture. The wet granulation was dried at a temperature below 60° C. until the moisture content was less than about 4%. The dried granulation was sized by passing it through a mill, and then blended with the additional ingredients listed in the table below using conventional mixing equipment. milled were added over about 10 minutes The wet granulation was dried at a temperature below 60° C. until the moisture content