A kind of color development method of hydrogen-containing hypophosphite

Abstract

The invention relates to a color developing method of hydrogen-containing phosphinate, which belongs to a selective color developing method of phosphinate in an organic reaction process. The method comprises the following steps: (1) color developing agent immersion: the color developing agent comprises 1g to 6g of phosphomolybdic acid, cerium ammonium molybdate or ammonium molybdate, dissolving the color developing agent into 5mL to 10mL of distilled water, adding 2mL to 10mL of concentrated hydrochloric acid, perchloric acid or concentrated sulfuric acid, making the volume to 100mL by utilizing acetone, water or ethanol, immersing an unfolded silicone sheet, and then taking out the silicone sheet; (2) drying, to be specific, drying the immersed sheet by utilizing a hot air mode of a dryer, and heating the sheet to the temperature of 100 to 150 DEG C, so that the color of the silicone sheet turns white from blue along with the increased temperature; and (3) iodine fumigation, to be specific, placing the dried sheet into an iodine cylinder, fumigating the sheet by iodine steam in the iodine cylinder to develop color, standing the sheet for 2 to 3 minutes, therefore, a clear dark blue color is displayed by the hydrogen-containing phosphinate, slight light blue is displayed by phosphate, and other ketones, acids, amines and carboxylic esters do not display color. The method has advantages that the sensitivity is high, convenience in operation is realized, rapidness in analysis is realized, and a good qualitative detection tool is provided for researching and developing the hydrogen-containing phosphinate compounds by combining the method with other color developing methods.

Description

technical field [0001] A selective color development method in an organic reaction process, specifically a color development method containing hydrogen hypophosphite. Background technique [0002] Thin-layer chromatography (TLC) is a technique commonly used in organic synthesis and is often used to track organic reactions and determine the progress of the reaction. For a simpler reaction, the product can be determined by comparing the Rf value of the raw material and the reaction mixture; for a more complex reaction, in addition to the target product, there are several by-products. How to determine the existence of the target product from the mixture and further separate and purify it is very important. difficulty. Ordinary color development methods are often untargeted, and all components in the mixture show the same color. If selective color development can be performed on the target product, the location of the target product can be identified, and then the subsequent se...

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Problems solved by technology

The Montchamp research group proposed to use ethanol (93%) concentrated sulfuric acid (3.5%) vanillin (2.5%) acetic acid (1%) chromogenic agent, but the chromogenic agent sensitivity is not high, when the solution concentration is thinner, the color development is extremely Weak; using this chromogen, the silica gel sheet shows blue, hydrogen-containing hypophosphite shows a darker blue, the difference between the background and the target is not obvious, and the color rendering effect is not clear; using this chromogen, phosphate compounds Also shows darker blue, less selective

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