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Gas chromatography detection method and preparation method of iodometyl pivalate

A technology of iodomethyl pivalate and a detection method, applied in the gas chromatography detection method of iodomethyl pivalate and the field of preparation thereof, can solve the problems of complicated operation, difficult application, high cost and the like, and achieve high product yield , good purity, fast response effect

Active Publication Date: 2017-12-01
SHANDONG YUXIN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The second object of the present invention is to provide a novel preparation method of iodomethyl pivalate, which overcomes the low yield and purity of iodomethyl pivalate prepared in the prior art, serious waste water pollution, cumbersome operation, and high cost. Difficulty and other issues

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  • Gas chromatography detection method and preparation method of iodometyl pivalate
  • Gas chromatography detection method and preparation method of iodometyl pivalate
  • Gas chromatography detection method and preparation method of iodometyl pivalate

Examples

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preparation Embodiment 1

[0109] Add 50ml of acetonitrile and 13.2g of sodium iodide to a 250ml single-necked bottle, stir and raise the temperature to 50°C, add 12g of pivaloyl chloride methyl ester, and react for 1h. The liquid was concentrated under reduced pressure at 20°C until a large amount of solids were precipitated, and 90 ml of dichloromethane was added for filtration. The filtrate was passed through a 30° C. falling film evaporator at 2 ml / min to obtain 18.5 g of iodomethyl pivalate with a yield of 95.9% and a product purity of 99.8%.

preparation Embodiment 2

[0111] Add 36ml of ethyl acetate and 15.0g of sodium iodide to a 250ml single-necked bottle, stir and raise the temperature to 40°C, add 12g of pivaloyl chloride methyl ester, and react for 3h. The liquid was concentrated under reduced pressure at 25°C until a large amount of solids were precipitated, and 72ml of dichloromethane was added for filtration. The filtrate was passed through a 40°C falling film evaporator at 2.5ml / min to obtain 18.2g of iodomethyl pivalate with a yield of 94.4% and a product purity of 99.8%.

preparation Embodiment 3

[0113] Add 72ml of acetone and 16.8g of sodium iodide to a 250ml single-necked bottle, stir and raise the temperature to 30°C, add 12g of pivaloyl chloride methyl ester, and react for 2h. Concentrate the liquid under reduced pressure at 30°C until a large amount of solid precipitates, add 100ml of dichloromethane and filter. The filtrate was passed through a 50° C. falling film evaporator at 3 ml / min to obtain 18.0 g of iodomethyl pivalate with a yield of 93.4% and a product purity of 99.7%.

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Abstract

The invention belongs to the technical field of pharmacochemistry, and particularly relates to a gas chromatography detection method and a preparation method of iodometyl pivalate. The detection method comprises the following steps of (1) storing a sample to be tested under the light avoiding and drying conditions; (2) setting the work conditions of a gas chromatograph, wherein a chromatographic column selects a KB-5 capillary chromatographic column; the column box temperature is 110 to 220 DEG C; the sampling opening temperature is 220 DEG C; the temperature of a detector is 240 DEG C; the flow rate of carrier gas is 0.3 to 0.7 ml / min; the split ratio is 80 to 1; the sampling quantity is 0.1mu L. By the preparation method of samples for detection, a treated iodometyl pivalate solution passes through a falling-film evaporator to obtain high-quality iodometyl pivalate. The analysis speed of the detection method is high; the detection sensitivity is high; the analysis result is accurate; no three wastes (waste water, waste gas and waste residue) are generated in the preparation process; the product purity is high.

Description

technical field [0001] The invention belongs to the field of pharmaceutical intermediates, in particular to a gas chromatography detection method of iodomethyl pivalate and a preparation method thereof. Background technique [0002] Iodomethyl pivalate, also known as iodomethyl pivalate, iodomethyl pivalate, is an important pharmaceutical intermediate with a boiling point of 197°C and a flash point of 73°C, insoluble in water but soluble in alcohol , ethers, ketones and other organic solvents. [0003] Its structural formula is: [0004] The gas chromatography detection method has the characteristics of fast analysis speed and can avoid the deterioration and decomposition of iodomethyl pivalate. At present, there are no relevant documents and detailed reports about the iodomethyl pivalate content assay method. [0005] Simultaneously, the preparation of iodomethyl pivalate is mostly made solvent with acetone, directly replaces the method with sodium iodide, and preparat...

Claims

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Application Information

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IPC IPC(8): G01N30/02C07C67/287C07C67/48C07C67/52C07C67/54C07C69/63
CPCC07C67/287C07C67/48C07C67/52C07C67/54G01N30/02C07C69/63
Inventor 刘振腾苏国王秀田管章委
Owner SHANDONG YUXIN PHARMA CO LTD
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