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Synthesis method of 2,5-diamino benzene ethanol

A technology of diaminobenzene and synthetic method, which is applied in two fields, can solve the problems of many diacetyl compounds, unfavorable industrial production, and low yield, and achieve the effects of stable and stable yield, increased product cost, and high yield

Active Publication Date: 2010-04-28
辽宁新宇生物科技有限公司
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Problems solved by technology

[0017] The shortcoming of this synthetic route is: in the nitration reaction, the by-product 2-amino-4-nitrophenylethanol diacetyl compound produced is more, and it is difficult to remove, resulting in a lower yield, which is unfavorable for industrial production

Method used

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  • Synthesis method of 2,5-diamino benzene ethanol
  • Synthesis method of 2,5-diamino benzene ethanol
  • Synthesis method of 2,5-diamino benzene ethanol

Examples

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Embodiment Construction

[0050] The present invention will be described in detail below in conjunction with specific embodiments.

[0051] 1) Synthesis of o-nitrophenylacetic acid

[0052] Add 220g (1.6mol) o-nitrotoluene, 375g sodium phenoxide, 85g sodium methoxide and 1500ml DMF to a 5000mL flask and heat to 45°C, pass through dry CO2 gas, cool at constant temperature for 35h, and hydrolyze with hydrochloric acid. Petroleum ether extraction, the extract was extracted with saturated sodium bicarbonate solution and acidified with hydrochloric acid. The product was washed with water, extracted with petroleum ether, and dried. The solvent was evaporated to obtain a product content > 99%, and a yield of 100%.

[0053] 2) Synthesis of o-aminophenylacetic acid

[0054] Dissolve 200g of o-nitrophenylacetic acid in 1 liter of methanol, and then add it to a 2 liter hydrogenation tank; add 5g of 5% pd / C catalyst at the same time. Replace with nitrogen for 3 times and then with hydrogen for 3 times, then int...

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Abstract

The invention discloses a synthesis method of 2,5-diamino benzene ethanol, which takes ortho-nitrotoluene as a starting material, and 2,5-diamino benzene ethanol is obtained by the processes of carboxylation, acetylation, nitration, esterification, reduction, hydrolyzation, hydrogenation and the like and the process of salifying with sulfuric acid finally. The process route has the advantages of easily obtained raw materials, mild reaction condition, high and stable yield, low cost, simple operation and the like, thereby being applicable to industrial production.

Description

technical field [0001] The invention relates to a method for preparing a compound, in particular to a method for synthesizing 2,5-diaminophenethyl alcohol. Background technique [0002] 2,5-diaminophenylethanol and its salt are mainly used as a kind of efficient oxidative hair dye, and its price is expensive, and there are few bibliographic reports about its synthesis. Various synthetic 2,5-diaminobenzene reported in domestic and foreign literature The method of ethanol can be roughly divided into two categories according to the difference of starting materials, and the specific methods are as follows: [0003] 1. Synthesize 2,5-diaminophenethyl alcohol with o-chlorophenylacetic acid as the starting material [0004] Taking o-chlorophenylacetic acid as the starting material to synthesize 2,5-diaminophenethyl alcohol has two different synthetic routes, which are specifically introduced as follows: [0005] Route 1: [0006] [0007] The temperature of this method is con...

Claims

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Application Information

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IPC IPC(8): C07C215/68C07C213/02
Inventor 袁顺福俞志平
Owner 辽宁新宇生物科技有限公司
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