Method for synthesizing 2-methyl-1,4-naphthaquinone by taking ionic liquid as catalyst

An ionic liquid and catalyst technology, applied in the field of synthesizing 2-methyl-1, can solve the problems of chromium-containing wastewater and serious environmental pollution, and achieve the effect of fast reaction speed

Inactive Publication Date: 2012-06-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The yield of oxidizing 2-methylnaphthalene with chromic anhydride (J.Bio.Chem.1940,133,391), dichromic acid (JP10245358) or Jones reagent (Tetrahedron Lett.2005,46,1091) is about 50~60 %, but the chromium-containing wastewater causes serious environmental pollution

Method used

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  • Method for synthesizing 2-methyl-1,4-naphthaquinone by taking ionic liquid as catalyst
  • Method for synthesizing 2-methyl-1,4-naphthaquinone by taking ionic liquid as catalyst
  • Method for synthesizing 2-methyl-1,4-naphthaquinone by taking ionic liquid as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Preparation of the first step ionic liquid

[0014] Stir equimolar pyridine (15.82g) and 1,4-butane sultone (27.23g) at room temperature for 3 days to obtain a white solid, wash with ethyl acetate to obtain a white solid ylide; then weigh equimolar The ylide (4.31g) and phosphoric acid (85%, 2.31g) were stirred and reacted at 80°C for 6h, and then rotary evaporated at 80°C for 4h to obtain the ionic liquid [SO 3 H-BPy][H 2 PO 4 ].

[0015] Synthesis of the second step 2-methyl-1,4-naphthoquinone

[0016] Add 0.05mol 2-methylnaphthalene, 0.25mol glacial acetic acid and 0.48mmol ionic liquid [SO 3 H-BPy][H 2 PO 4 ], when the above reactants were heated to 90°C, 20ml H 2 o 2 (30%, H 2 o 2 0.2 mol) was added dropwise in 20 minutes, and the temperature was maintained for 2 hours. During the reaction, samples were taken regularly for GC-MS qualitative and GC quantitative analysis, and the yield was 61%.

Embodiment 2-4

[0018] Except that following and catalyst (0.64mmol) are different, all the other are identical with embodiment 1, H 2 o 2 Dosage according to Table 1.

[0019] Table 1

[0020]

Embodiment 5-7

[0022] Except that following and catalyst (0.64mmol) are different, all the other are identical with embodiment 1, and HAOc consumption is by table 2 consumption.

[0023] Table 2

[0024]

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Abstract

The invention discloses a method for synthesizing 2-methyl-1,4-naphthaquinone by taking ionic liquid as a catalyst. The method comprises the following steps of: adding 2-methylnaphthalene, acetic acid and ionic liquid acidified by phosphoric acid into a reaction container provided with a magnetic stirrer and a thermometer, heating for reaction; adding H2O2 (30%) in a dripping way when the reactant is heated to the temperature of 60-100 DEG C; reacting for 2h after finishing dripping; and directly washing and filtering the reaction solution, thus obtaining 2-methyl-1,4-naphthaquinone. The method adopts ionic liquid as the catalyst for the first time, has the advantages of high conversion rate of 2-methylnaphthalene, less using amount of the catalyst, fast reaction speed, no chromic waste liquor pollution, and the like.

Description

technical field [0001] The invention relates to the technical field of fine chemical synthesis, in particular to a method for synthesizing 2-methyl-1,4-naphthoquinone with an ionic liquid as a catalyst. Background technique [0002] 2-Methyl-1,4-naphthoquinone (2-Methyl-1,4-naphthoquinone) is an important compound, which is the earliest used vitamin K3 and a key intermediate in the synthesis of vitamin K, which can be used together with vitamin C It is used for the treatment of tumor patients, and the effect is remarkable; it can also be used as a feed additive; it can also be used as a coating for ships, warships, etc., and it has a wide range of uses. Therefore, the synthesis technology of 2-methyl-1,4-naphthoquinone has been paid much attention. [0003] There are many methods for the preparation of 2-methyl-1,4-naphthoquinone, which are roughly divided into two types: direct oxidation method and indirect conversion method. Direct oxidation methods include 2-methylnapht...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C50/12C07C46/04B01J31/02
Inventor 杨建国权南南鲍少华张敬朱娟陈露
Owner EAST CHINA NORMAL UNIV
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