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Preparation method of 2-methyl-1-phenyl-1-propanol

A phenyl and methyl technology, applied in the field of preparation of organic compound 2-methyl-1-phenyl-1-propanol, can solve the problems of reduced reaction selectivity, difficult preparation of catalysts, difficult industrial application, etc. The effect of avoiding the use of catalyst, good industrial application value and convenient post-processing

Inactive Publication Date: 2018-12-18
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalyst of this method is difficult to prepare, the required reaction temperature is very low, it is difficult to apply industrially, and the yield is only 85%.
In this method, if the -78°C is adjusted to -20~10°C, the by-products will increase (such as biphenyl, terphenyl), and the reaction selectivity will be greatly reduced.

Method used

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  • Preparation method of 2-methyl-1-phenyl-1-propanol
  • Preparation method of 2-methyl-1-phenyl-1-propanol
  • Preparation method of 2-methyl-1-phenyl-1-propanol

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Embodiment 1

[0041] The preparation method of embodiment 1,2-methyl-1-phenyl-1-propanol, carries out following steps successively:

[0042] 1) Take a 500ml three-neck flask, add 13.2g (0.55mol) of magnesium chips, 200ml of tetrahydrofuran and 0.66g of zinc-sodium alloy as an additive, turn on nitrogen purge to replace the air, and heat up to reflux (65°C). Take 56.280 g (0.5 mol) of chlorobenzene in a constant pressure dropping funnel, and slowly drop it into the flask under nitrogen protection (0.5 h for dropping), after 2.5 h of reaction, sample GC to detect that the chlorobenzene has reacted completely.

[0043] 2) Under the protection of nitrogen, take 36.055g (0.5mol) of isobutyraldehyde and slowly drop it into the flask in a constant pressure dropping funnel (the time for dropping is 0.5h). Magnesium chloride has reacted completely.

[0044] 3), the obtained reaction solution is filtered, and the obtained filter residue is excessive magnesium, and 0.724 g of magnesium scraps are rec...

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Abstract

The invention discloses a preparation method of 2-methyl-1-phenyl-1-propanol, and the method comprises the steps of: adding magnesium chips and additives to an organic solvent under the protection ofan inert gas, heating to reflux, further adding dropwise chlorobenzene for reaction under reflux conditions, and adding dropwise isobutyraldehyde to continue the reaction under the reflux conditions;filtering an obtained reaction solution to recover the magnesium chips, adding an acid solution or a weak acid salt aqueous solution into filtrate for hydrolysis, allowing an obtaining reaction liquidto stand for liquid separation, collecting an organic phase, recovering the organic solvent from the organic phase, and distilling under a reduced pressure to obtain the 2-methyl-1-phenyl-1-propanol.The method has a high raw material utilization rate, the use of a high-cost catalyst is avoided, three wastes are reduced, the production cost is lowered, the product purity is high, the yield is high, and the product has good industrial application value.

Description

technical field [0001] The present invention relates to the preparation method of organic compound 2-methyl-1-phenyl-1-propanol. Background technique [0002] 2-Methyl-1-phenyl-1-propanol is an important fine chemical intermediate, mainly used in photoinitiators (such as photoinitiator 1173, 2-hydroxy-2-methyl-1-phenyl -1-acetone), pharmaceutical intermediates, synthesis of material intermediates, etc. [0003] The preparation methods currently reported for 2-methyl-1-phenyl-1-propanol are: [0004] 1. Patent EP 718265 etc. proposed isobutyrophenone reduction method. This method is synthesized by reducing isobutyrophenone with high-pressure hydrogen under the catalysis of noble metals. The reaction raw materials of this method are difficult to obtain, the use cost of the catalyst is high, and the high-pressure hydrogen operation requires high equipment. [0005] 2. Grignard reagent synthesis method. Literature (Chemical Communications, 2017,53(79):10942-109445) proposes...

Claims

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Application Information

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IPC IPC(8): C07C29/68C07C29/70C07C29/09C07C33/20C07F3/06C07F3/02
CPCC07C29/09C07C29/68C07C29/70C07C33/20C07F3/003
Inventor 陈新志徐泽钱超
Owner ZHEJIANG UNIV
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