The relation between natural and synthetical glycerylphosphoric acids. Pt. 2 / by Frank Tutin and A.C.O. Hann.
- Tutin, Frank.
- Date:
- [1906]
Licence: In copyright
Credit: The relation between natural and synthetical glycerylphosphoric acids. Pt. 2 / by Frank Tutin and A.C.O. Hann. Source: Wellcome Collection.
8/14 page 1754
![0*2048 of salt, dried at 100°, gave 0*4591 CO., and 0*1143 H09. 0—61*1 ; H = 6*2. “ . C49H6i0i4N4P,9H20 requires C = 52*4 ; 14 = 6-9 ; H20 = 14*4 per cent. C49Hgi014N4P r©4nires 0 = 61*3 ; 11 = 6*3 per cent.* 1/ The specific rotation of the salt dried at 100° was determined in aqueous and in alcoholic solution. 0*2178, dissolved in 25 c.c. of absolute alcohol, gave aD -34' in a 2-dcm. tube, whence [a]D-32*5°. 0*1608, dissolved in 25 c.c. of water, gave aD — 19*5' in a 2-dcm. tube, whence [a]D - 25*3°. /0*ch:(oh2*oh)2 p-Glycerylphosphoric A cid, 0 = Py—OH H)H (a) Preparation of Calcium ft-Diglycerylphosphate, 4>oh:(ch2-oh)9 4>ch:(ch2*oh)2 (cir2-on)2:cH-o> 0 ^o-ch:(ch2-oh) (CH2-OH)2:cH-cr u ° u The a-dichlorohydrin required for this preparation was obtained from Kahlbaum, and was submitted to a careful fractionation. Only the portion boiling from 173—176° was employed, which was found to be pure. Equivalent molecular proportions of a-dichlorohydrin and phosphoryl chloride were boiled together in a round-bottomed flask attached to a reflux condenser, when a copious evolution of hydrogen chloride ensued. At the end of two and three-quarter hours the dark liquid was poured into a large excess of milk of lime, the mixture boiled for two hours in a flask attached to a reflux condenser, then filtered, and the excess of lime removed from the filtrate by means of carbon dioxide. On evaporating the filtrate, the crude calcium /?-diglycery]phospliate, which separated as a scum on the surface of the liquid, was removed from time to time and dried on a porous tile. From 50 grams of the dicblorohydrin about 18 grams of crude calcium salt were obtained. When crystallised from water, calcium /3-di- glycerylphosphate was obtained in long, slender needles, which melted at 249—250°. It dissolves very readily in alcohol and in ethyl acetate, but less readily in water, chloroform, or benzene ; it is insoluble in light petroleum. When the crystallised salt is heated, it suffers a decrease in weight, but it was found impracticable to estimate the water of crystallisation by this method, as the temperature necessary for complete dehydration also causes gradual decomposition. 0*3081 of air-dried salt gave 0*0230 CaO. Ca = 5*3. The air-dried salt was then analysed in the usual manner. * One atom of hydrogen becomes fixed as HP03.](https://iiif.wellcomecollection.org/image/b30610035_0008.jp2/full/800%2C/0/default.jpg)
