Method for preparing 3-methyl-3-buten-1-ol

A technology of butene and methyl is applied in the field of preparation of water reducing agent intermediates, which can solve the problems of difficulty in storage and transportation of raw materials, harsh process conditions, etc., and achieves the effect of simple process and easy storage.

Inactive Publication Date: 2013-01-02
JIANGSU SOBUTE NEW MATERIALS +2
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  • Abstract
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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the current preparation method of 3-methyl-3-buten-1-ol, such as harsh requirements on process conditions, difficulties in storage and transportation of raw materials, etc. Process for preparing 3-methyl-3-buten-1-ol

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  • Method for preparing 3-methyl-3-buten-1-ol
  • Method for preparing 3-methyl-3-buten-1-ol

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 80mL of anhydrous tetrahydrofuran to a 500mL three-necked flask equipped with magnetic stirring, constant pressure dropping funnel and reflux condenser, then add 7.84g (0.327mol) of polished magnesium chips, and then add 0.254g (0.001mol) Iodine, blow nitrogen, add 0.327g (0.003mol) ethyl bromide dropwise at room temperature, wait until the color of the mixture becomes lighter and the reaction starts, add 100mL tetrahydrofuran and 30mL (0.297mol) methallyl Chlorine solution, the temperature of the reaction mixture is controlled below 40°C during the dropwise addition. After the dropwise addition, continue to react for 2h, then add 9.36g (0.104mol) of paraformaldehyde (n=3), raise the temperature to 60°C, react for 2.5h, then cool to room temperature, add dropwise 200mL of saturated ammonium chloride solution to three ports The product was hydrolyzed in a flask, the obtained aqueous layer was extracted 3 times with anhydrous ether, the obtained organic phase was drie...

Embodiment 2

[0029] Add 150mL of anhydrous diethyl ether to a 1000mL three-necked flask equipped with magnetic stirring, constant pressure dropping funnel and reflux condenser, then add 14.11g (0.588mol) of polished magnesium chips, and then add 0.762g (0.003mol) Iodine, blow argon, drop 0.436g (0.004mol) ethyl bromide at room temperature, wait until the color of the mixed solution becomes lighter, that is, after the reaction starts, add 150mL ether and 50mL (0.511mol) methallyl dropwise The temperature of the reaction mixture is controlled below 40°C during the dropwise addition. After the dropwise addition, continue to react for 1 hour, then add 16.86g (0.562mol) formaldehyde (n=1), raise the temperature to 40°C, react for 3 hours, cool to room temperature, add dropwise 250mL saturated ammonium chloride solution to the three-necked flask to test the product Carry out hydrolysis, the obtained aqueous layer is extracted 3 times with anhydrous ether, the obtained organic phase is dried with...

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Abstract

The invention relates to a method for preparing 3-methyl-3-buten-1-ol, which comprises the following steps: adding magnesium chips into an anhydrous solvent under the protection of inert gas, then adding bromoethane to initiate the reaction; after the color of the mixed solution is light, adding methallyl halide to carry out Grignard reaction so as to prepare a Grignard reagent; adding formaldehyde or paraformaldehyde into the Grignard reagent to perform addition reaction; then performing after-treatment to obtain 3-methyl-3-buten-1-ol. According to the method provided by the invention, rigorous requirements on the process condition and difficult storage and transportation problems of the adopted raw material in the prior art are overcome, the raw materials suitable for storage and transportation are adopted, and the process is simple.

Description

technical field [0001] The invention relates to a method for preparing a water reducer intermediate, belonging to the technical field of fine chemicals. Background technique [0002] 3-Methyl-3-buten-1-ol (MBOH) is an important intermediate in organic synthesis, and its latest development is for the synthesis of polycarboxylate concrete water reducers and low-toxicity, high-efficiency Pyrethroid insecticides. The functional macromonomer synthesized by using this raw material plays a decisive role in the quality and performance of polycarboxylate superplasticizer products, making it have a strong ability to maintain the dispersion of cement particles, low dosage, and high water reducing rate. , good reinforcement effect, durability, non-corroding steel bars and environmental friendliness. At present, the market demand for the third-generation polycarboxylate concrete superplasticizer with 3-methyl-3-butene-1-ol as the starting material is huge, while domestic 3-methyl-3-but...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/10
Inventor 王涛冉千平杨勇范士敏吕志峰刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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