ChemicalBook CAS DataBase List 2-Methyl-5-vinylpyridine

2-Methyl-5-vinylpyridine synthesis

6synthesis methods

Product Name:2-Methyl-5-vinylpyridine
CAS Number:140-76-1
Molecular formula:C8H9N
Molecular Weight:119.16

53014-84-9 Synthesis

53014-84-9
187 suppliers
$19.00/1g

1779-49-3
603 suppliers
$5.00/10g

140-76-1
144 suppliers
$21.00/250mg

Yield: 38.2 g

Reaction Conditions:

Stage #1:Methyltriphenylphosphonium bromide with potassium tert-butylate in diethyl ether at 5; for 1 h;
Stage #2:2-methyl-5-formylpyridine in diethyl ether at 10; for 0.5 h;Solvent;

Steps:

1.2; 1.3 Example 1
2) Take 173g of methyl bromide triphenyl phosphate put in2L four bottles,Add 400ml ether organic solvent,When the bottle dissolvedThe agent temperature is reduced to below 5 after adding batches of potassium tert-butoxide 57g, after the reaction was continued stirring 1h standby;3) The reaction solution obtained in 1) was slowly added dropwise to 2)Control the drop acceleration,The reaction temperature of the reaction liquid will rise,The temperature can not exceed 10 ,To be added dropwise after the reaction was continued for 30min,The reaction was fully carried out, and the reaction solution was sufficiently reacted.The reaction product, triphenylphosphine, was filtered off,The filtrate was concentrated under reduced pressure at 80 ° C and the distillate was collected by distillation at 110 to 130 ° C to obtain the product.Vacuum concentrated vacuum ≤ 0.08MPa,Distillation was added methyl hydroquinone 1g as a polymerization inhibitor, a total of 38.2g product, the total yield of 74.9%.Gas chromatographic analysis of the product of Example 1, the chromatograph modelN2000, and the chromatographic integration method is the area normalization method. Referring to the gas chromatogram of Example 1 of FIG. 1 and the chromatographic analysis result of FIG. 2, it can be seen from the test results that the purity of the product GC obtained by the method of the present invention reaches more than 99% The present invention is effectiveReduce the formation of by-products, high reaction yield brings convenience to subsequent processing, making the purity of products reach the ideal standard.

References:

Xi'an Tianyi Bio-technology Co., Ltd.;Yao Weibang;Wang Xiao CN106349153, 2017, A Location in patent:Paragraph 0033; 0036; 0037; 0041; 0042; 0046; 0047; 0051

3430-13-5 Synthesis