dried over Drierite and fractionated through a column 10 in. long, 1/i in. in diameter and packed with a tantalum spiral. The fraction boiling at 42.2°at 38 mm. weighed 1.12 g., n2SD 1.5774, d254 2.3853; molar refractivity caled. 29.35, found 29.31. Auger reported b.p. 131°at 760 mm., ¿»4 2.41.d Kinetic Runs.-All runs were made in 100-ml. volumetric flasks in a constant temperature bath maintained at 35.0 ± 0.1°. Chloroform was introduced into the reaction vessels by the use of a 0.25-ml. "tuberculin" syringe graduated in 0.01 ml. and found to deliver 0.250 ml. with an average deviation of 0.002 ml. The runs were carried out by dissolving 0.250 ml. of chloroform (at a known temperature)
Polychloral diol, unlike polyoxymethylene diol, is not readily capped in the presence of alkali catalysts. Polychloral is capped under acid conditions by acid anhydrides and chlorides and does not appear to undergo degradation during the process. Evidence for end‐capping is provided by infrared analysis in the case of the low DP polychloral, metachloral. End‐capped polychlorals possess good stability towards hot dimethylformamide and good stability at elevated temperatures (255°C.). From the melting points of copolymers, polychloral itself is estimated to have a melting point of about 460°C. The high melting point is consistent with the rigidity of the polymer chain. A means of estimating the DP of the polymer is proposed, based on a form of endgroup analysis. By this technique, metachloral is estimated to have a DP of about 50.
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