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Preparation method for 2-alkyl-cyclopentanone (cyclohexanone) by using tert-butyl peroxybenzonate

A technology for tert-butyl peroxybenzoate and alkylcyclopentadiene is applied in the field of preparation of 2-alkylcyclopentanone by one-step method, which can solve problems such as unsatisfactory reaction yield, and achieve high yield and low yield. The effect of less cost and three wastes

Active Publication Date: 2014-03-19
北京北达正元科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The two-step and three-step methods have certain limitations in industrial applications due to the many disadvantages and limitations mentioned above
Regarding the one-step method, although the predecessors have also done some research, all the research only stays at a certain stage, and only studies the influence of temperature on the reaction yield, and the reaction yield is not very ideal in essence.

Method used

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  • Preparation method for 2-alkyl-cyclopentanone (cyclohexanone) by using tert-butyl peroxybenzonate
  • Preparation method for 2-alkyl-cyclopentanone (cyclohexanone) by using tert-butyl peroxybenzonate
  • Preparation method for 2-alkyl-cyclopentanone (cyclohexanone) by using tert-butyl peroxybenzonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: Synthesis of 2-pentylcyclopentanone

[0042] Synthesis was carried out using 1,1-di-tert-butylperoxycyclohexane (the purity of which is 80%, the same applies hereinafter) as an initiator. In the reaction flask equipped with stirring reflux device and temperature measurement, add 80 grams (0.95 moles) of cyclopentanone, 8 grams (0.023 moles) of 1,1-di-tert-butylperoxycyclohexane, stir and heat, reflux state Add 7 grams (0.1 mole) of 1-pentene within 5 hours, continue to reflux reaction for 6 hours, recover excess cyclopentanone, and rectify under reduced pressure to obtain 11.5 grams of a product with a content of 99%.

[0043] Yield=(11.5 / 154) / 0.1×100%=74.7%

[0044] The ratio of raw materials and the yield of products are summarized in Table 1.

Embodiment 2

[0045] Embodiment 2: Synthesis of 2-pentyl cyclopentanone

[0046] The synthesis was carried out using tert-butyl peroxybenzoate (the purity of which is 75%, the same applies hereinafter) as an initiator. In the reaction flask equipped with stirring reflux device and temperature measurement, add 80 grams (0.95 moles) of cyclopentanone, 5 grams (0.019 moles) of tert-butyl peroxybenzoate, stir and heat, add 7 Gram (0.1 mole) 1-pentene, after adding, continue to reflux reaction for 7 hours, recover excess cyclopentanone, and rectify under reduced pressure to obtain 11.8 grams of product with a content of 99%, yield 76.6%. The ratio of raw materials and the yield of products are summarized in Table 1.

Embodiment 3

[0049] Embodiment 3: Synthesis of 2-pentylcyclohexanone

[0050] In the reaction flask equipped with a stirring reflux device and temperature measurement, add 98 grams (1 mole) of cyclohexanone, 5 grams (0.019 moles) of tert-butyl peroxybenzoate, stir and heat, and add 7 Gram (0.1 mole) 1-pentene, after the addition, the reflux reaction was continued for 6 hours, and excessive cyclopentanone was recovered, followed by rectification under reduced pressure to obtain 12.8 grams of a product with a content of 99%, with a yield of 76.2%. The ratio of raw materials and the yield of products are summarized in Table 1.

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Abstract

The invention provides a preparation method for 2-alkyl-cyclopentanone (cyclohexanone) by using tert-butyl peroxybenzonate. The method is characterized in that: cyclopentanone (cyclohexanone) is used as a raw material, through a free radical reaction, cyclopentanone (cyclohexanone) and alkene undergo addition under the action of tert-butyl peroxybenzonate functioning as an initiator, so 2-alkyl-cyclopentanone (cyclohexanone) is prepared in one-step, wherein, the number of carbon atoms in the alkene is 3 to 15. The preparation method for synthesis of 2-alkyl-cyclopentanone (cyclohexanone) in the invention has the advantages of high yield, low cost, production of a high purity product, short process flow and accordance with clean production.

Description

[0001] This application is a divisional application of the Chinese patent application whose filing date of the original application is June 10, 2009, the application number is 2009100871514, and the title of the invention is "Preparation Method of 2-Alkylcyclopenta(hexanone)". technical field [0002] The present invention relates to the preparation method of 2-alkylcyclopent(hexanone) ketone. In particular, it relates to a preparation method for obtaining 2-alkylcyclopent(hexanone) in one step. Background technique [0003] There are three main methods for preparing 2-substituted cyclopentanone (hexanone) as follows. [0004] The first is a two-step method. That is, using cyclopentyl (hexanone) ketone represented by the following formula (I) as a raw material, condensing with aliphatic aldehyde to generate 2-alkenyl cyclopentyl (hexyl) ketone represented by the following formula (II), and then catalytic hydrogenation to generate 2-substituted cyclopentan(hexanone) represe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/395C07C49/403C07C45/69
Inventor 王川卫小广
Owner 北京北达正元科技有限公司