1943
DOI: 10.1021/i560115a023
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Microdeterminination of Hydroxyl Content of Organic Compounds - Acetic Anhydride-Pyridine Mixture as Reagent

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Cited by 32 publications
(8 citation statements)
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“…The method most frequently used for the determination of hydroxyl groups, which was first proposed in 1901 by Verley and Bolsing (23), is esterification by acetic anhydride in pyridine solution. More recent modifications by this method are described by Ogg, Porter, and Willits (12) and Christensen and his co-1 Present address, Purdue University, Lafayette, Ind, 5Present address, Camp Detrick, Frederick, Md. workers (13). While this method has been successfully applied to the determination of most primary alcohols and many secondary alcohols, it is not readily applied to volatile compounds; aldehydes, especially those of relatively low molecular weight, interfere by reacting with the acetic anhydride; phenols react partially or completely, interfering with the direct determination of the alcoholic hydroxyl content of the sample; and the presence of more than a small amount of water in the sample renders the determination inexact or impossible (20).…”
Section: Inmentioning
confidence: 99%
“…The method most frequently used for the determination of hydroxyl groups, which was first proposed in 1901 by Verley and Bolsing (23), is esterification by acetic anhydride in pyridine solution. More recent modifications by this method are described by Ogg, Porter, and Willits (12) and Christensen and his co-1 Present address, Purdue University, Lafayette, Ind, 5Present address, Camp Detrick, Frederick, Md. workers (13). While this method has been successfully applied to the determination of most primary alcohols and many secondary alcohols, it is not readily applied to volatile compounds; aldehydes, especially those of relatively low molecular weight, interfere by reacting with the acetic anhydride; phenols react partially or completely, interfering with the direct determination of the alcoholic hydroxyl content of the sample; and the presence of more than a small amount of water in the sample renders the determination inexact or impossible (20).…”
Section: Inmentioning
confidence: 99%
“…After temperature equilibration, from 8 to 16 "points" were determined in an experiment. Each of the 8 to 16 "points" was the average observed rotation at the average time of 4 to 7 readings taken over a time interval of 4-10 minutes.…”
mentioning
confidence: 99%
“…Deionized water (800 mL) was added and the crude acetoxy intermediate (compound 2) was precipitated and separated. 39 Compound 2 (1.5 mmol) was dissolved in N,N-dimethylformamide (1 mL) and thionyl chloride (10 mL), and stirred at 70 C for 5 min. Through distillation under reduced pressure, the liquid residue was collected and dispersed in 20 mL of CH 2 Cl 2 , to which 2-aminobenzothiazole (1.0 mmol) was added, and stirred at 0-5 C. The pH value was kept between 6 and 7 by addition of NaHCO 3 to induce precipitation.…”
Section: Synthesis Of Compound Q1-q4mentioning
confidence: 99%