PREPARATION OF INOSITE MONOPHOSPHORIC ACID. 



Wheat bran is digested in 0.2 per cent, hydrochloric acid over night. 

 Strain through cheesecloth and filter the extract. Add about 4 volumes of 

 95 per cent, alcohol, allow the precipitate to settle and then filter on a 

 Buchner funnel and wash with dilute alcohol. Dissolve the precipitate 

 in 0.2 per cent, hydrochloric acid, filter through a heavy layer of paper 

 pulp on a Buchner funnel and precipitate with 4 volumes of alcohol. 

 These operations are repeated six times or until a nearly white product 

 is obtained which dissolves in the dilute acid, giving a perfectly clear 

 solution. The substance is then dried in vacuum over sulfuric acid. 

 Dissolve it in water with the aid of a few drops of hydrochloric acid 

 and precipitate the solution with a concentrated solution of pure barium 

 hydroxide. Filter off the precipitate and wash with cold water. Evap- 

 orate the filtrate to about one-fourth its volume, remove the excess of 

 barium hydroxide with carbon dioxide, filter and evaporate the filtrate 

 to a thin syrup on the water bath. Pour the syrupy residue into a large 

 volume of 95 per cent, alcohol. Filter off the precipitate and dry it in 

 vacuum over sulfuric acid. Dissolve the dry substance in water and re- 

 precipitate with a large volume of alcohol. Filter, wash with alcohol 

 and dry as before. There is then obtained a nearly wh'te amorphous 

 powder. One preparation obtained in this way had the following com- 

 position : 



C = 39.22 ; H = 5.43 ; N = 14.26 ; Amino N (by Van Slyke method) 

 = 0.99; organic Phosphorus = 0.87 ; Ba =10.43 per cent. 



The crude nitrogen-containing substance was dissolved in water and 

 a concentrated solution of lead acetate added in excess. The resulting 

 precipitate was filtered, washed thoroughly in cold water and then sus- 

 pended in hot water and decomposed with hydrogen sulfide. The lead 

 sulfide was filtered off and the filtrate boiled to expel hydrogen sulfide. 

 The solution was then strongly acid to litmus and it had a sharp acid 

 taste. It was again precipitated as above three times with lead acetate. 

 The pure white colored lead precipitate wlvch was finally obtained was 

 decomposed with hydrogen sulfide. The filtrate was concentrated in 

 vacuum at a temperature of 40 to 45° and then dried in vacuum over 

 sulfuric acid until a thick, practically colorless syrup remained. On 

 scratching with a glass rod this immediately began to crystallize, form- 

 ing a white, solid mass. It was very soluble in water, but insoluble in 

 alcohol. It was extracted several times with 95 per cent, alcohol, fil- 

 tered and washed in absolute alcohol and ether and allowed to dry in the 

 air. For recrystallization it was dissolved in a small quantity of water 

 and absolute alcohol added until the solution turned slightly cloudy. On 

 scratching, the substance began to crystallize. After standing in the 

 ice chest over night it had separated in large, colorless plates or prisms 

 arranged in star-shaped aggregates. It was recrystallized a second time 

 in the same manner. 



34 



