- Method for synthesizing 3-methylindole through continuous flow reaction
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The invention provides a method for synthesizing 3-methylindole through a continuous flow reaction. The synthesis method comprises the steps of mixing and throwing a phenylhydrazine solution and a propionaldehyde solution into a first reaction module separately through a metering pump, wherein the standing time is 3-20 min, and the reaction temperature is 25-75 DEG C; phenylhydrazone is prepared through a reaction, and then when reaction liquid containing phenylhydrazone flows out of the first reaction module, and the metering pump connected with a ZnCl2 solution is started, so that the ZnCl2 solution and the reaction liquid containing phenylhydrazone is mixed and enters a second reaction module which is preheated to 150-200 DEG C, wherein the standing time is 4-10 min, and then reaction liquid which flows out of the second reaction module enters a collection device through a cooling pipe to be preprocessed to obtain the product 3-methylindole. The method for synthesizing 3-methylindole through the continuous flow reaction is high in reaction speed, less in side reaction, high in heat and mass transfer efficiency, high in reaction selectivity, high in purity and high in yield and convenient in aftertreatment, and meanwhile, expensive ionic liquid can be recycled and applied in a re-extraction mode.
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Paragraph 0026-0029; 0034-0037; 0042-0045; 0050; 0051
(2017/09/01)
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- Visible light-mediated C-H difluoromethylation of electron-rich heteroarenes
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A novel method for visible-light photoredox-catalyzed difluoromethylation of electron-rich N-, O-, and S-containingheteroarenes under mild reaction conditions is developed. Mechanistic investigation indicates that the net C-H difluoromethylation proceeds through an electrophilic radical-type pathway.
- Su, Yi-Ming,Hou, Yu,Yin, Feng,Xu, Yue-Ming,Li, Yan,Zheng, Xiaoqi,Wang, Xi-Sheng
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supporting information
p. 2958 - 2961
(2014/06/23)
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- Novel 1,5,3-dithiazepanes: Three-component synthesis, stereochemistry, and fungicidal activity
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Three-component heterocyclization of hydrazine with formaldehyde and ethane-1,2-dithiol gave previously unknown 3,3′-bi(1,5,3-dithiazepane). Its stereochemistry was determined by X-ray diffraction. The reaction with higher aliphatic aldehydes RCHO (R = Me
- Akhmetova,Murzakova,Tyumkina,Khabibullina,Bushmarinov,Korzhova,Galimzyanova
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p. 2140 - 2148
(2013/10/01)
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- Optodynamers: Expression of color and fluorescence at the interface between two films of different dynamic polymers
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Color and fluorescence changes were expressed at the interface between two different polyhydrazone polymer films, induced by hydrazone bond exchange and component recombination through the interface, resulting in an extension of conjugation. The Royal Society of Chemistry.
- Ono, Takashi,Fujii, Shunsuke,Nobori, Tadahito,Lehn, Jean-Marie
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p. 4360 - 4362
(2008/04/01)
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- Reactions of Glyoxals with Hydrazones: A New Route to 4-Hydroxypyrazoles
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N-Substituated hyrazones of aldehydes react with glyoxals under non-aqueous conditions to give N-substituted 4-hydroxypyrazoles; fourteen such products are described.In the presence of water, N-substituted 3-acyl-4-hydroxypyrazoles are produced from 2-oxoaldehyde hydrazones and glyoxals.It is shown that glyoxals combine in a 1:1 ratio with N-monosubstituted hydrazones to give 2-hydrazonoaldehydes as the kinetically controlled products.At room temperature or lower, these hydrazonoaldehydes rearrange to the more stable 2-oxoaldehyde hydrazones and react with glyoxals to give N-substituted 3-acyl-4-hydroxypyrazoles; sixteen such products are described.This synthesis, involving easily accessible starting materials, opens up a new, and for certain derivatives exclusive, route to 4-hydroxypyrazoles.
- Begtrup, Mikael,Nytoft, Hans Peter
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- ALKALINE ISOMERIZATION OF PHENYLHYDRAZONES TO ALKYLPHENYLDIIMIDES
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When solutions pf phenylhydrazones in tri- or tetraethylene glycol are heated in the presence of the corresponding sodium glycolate, they undergo isomerization to alkylphenyldiimidates.There is a marked decrease in the isomerization rate in the transition from the hydrazones of aldehydes to the hydrazones of ketones.With the phenylhydrazones of ketones the reaction takes place almost unambiguously, but in the case of hydrazones of aldehydes it is complicated to an appreciable extent by side processes such as indolization and aminonitrile cleavage.
- Kuznetsov, M.A.,Suvorov, A.A.
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p. 1684 - 1691
(2007/10/02)
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