Preparation method of cetomacrogol 1000

A polyethylene glycol and drying technology, which is applied in the preparation field of Situ Mage 1000, can solve the problems of Situ Mage 1000 industrial production difficulties, harsh storage and transportation conditions of ethylene oxide, and low safety, so as to avoid Inflammable and explosive, easy to operate and safe, high security effect

Inactive Publication Date: 2019-02-19
汕头经济特区鮀滨制药厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Most domestic enterprises adopt the above-mentioned process, but because in the above-mentioned industrial classic process method, ethylene oxide is a gas, flammable and explosive, and belongs to a class of carcinogens, and high-voltage equipment is required in the synthesis process, and explosion-pr

Method used

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  • Preparation method of cetomacrogol 1000
  • Preparation method of cetomacrogol 1000
  • Preparation method of cetomacrogol 1000

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The preparation method of embodiment 1 Situ Ma Ge 1000

[0032] (1) Polyethylene glycol 800 (157.50g, 191.61mmol, 1eq) was dissolved in dry tetrahydrofuran (2L), under nitrogen protection, and metal sodium (4.85g, 210.77mmol, 1.1 eq), heated to reflux for 20h.

[0033] (2) The reaction solution was cooled to room temperature, and hexadecane bromide (64.36 g, 210.77 mmol, 1.1 eq) was added dropwise. After the addition was complete, the mixture was heated under reflux for 20 h.

[0034] (3) The reaction liquid was cooled to room temperature, filtered, and the filtrate was concentrated to dryness to obtain the crude product of Situmage 1000.

[0035] (4) Dissolve the crude product of Situmage 1000 in ethyl acetate (100mL), add dropwise n-heptane (1000mL), stir at room temperature overnight, after the solid precipitates, filter and dry in vacuum to obtain Situmage 1000 (122.00g) , the yield of West Macco 1000 was 55%.

[0036] Wherein, the heating temperature of the heat...

Embodiment 2

[0037] The preparation method of embodiment 2 Situ Mage 1000

[0038] (1) Polyethylene glycol 800 (157.50g, 191.61mmol, 1eq) was dissolved in dry dichloromethane (2L), under nitrogen protection, and metal sodium (4.85g, 210.77 mmol, 1.1eq), heated at reflux at 45°C for 20h.

[0039] (2) The reaction solution was cooled to room temperature, and hexadecane bromide (64.36 g, 210.77 mmol, 1.1 eq) was added dropwise. After the addition was complete, the mixture was heated under reflux at 45° C. for 20 h.

[0040] (3) The reaction liquid was cooled to room temperature, filtered, and the filtrate was concentrated to dryness to obtain the crude product of Situmage 1000.

[0041] (4) Dissolve the crude product of Situmage 1000 in ethyl acetate (100mL), add dropwise n-heptane (1000mL), stir at room temperature overnight, after the solid precipitates, filter and dry in vacuo to obtain Situmage 1000 (110.28g) , yield 49.7%.

[0042] In this embodiment, the solvent used is dichlorometha...

Embodiment 3

[0045] The preparation method of embodiment 3 Situ Ma Ge 1000

[0046] (1) Polyethylene glycol 1000 (190g, 190mmol, 1eq) was dissolved in dry tetrahydrofuran (2L), under nitrogen protection, and metal sodium (4.85g, 210.77mmol, 1.1eq) cut into small pieces was added under stirring at room temperature , Heated to reflux at 70°C for 20h.

[0047] (2) The reaction solution was cooled to room temperature, and hexadecane bromide (64.36 g, 210.77 mmol, 1.1 eq) was added dropwise. After the addition was complete, the mixture was heated under reflux at 70° C. for 20 h.

[0048] (3) The reaction liquid was cooled to room temperature, filtered, and the filtrate was concentrated to dryness to obtain the crude product of Situmage 1000.

[0049] (4) The crude product of Situmage 1000 was dissolved in ethyl acetate (100mL), added dropwise with n-heptane (1000mL), stirred overnight at room temperature, after the solid precipitated, filtered, and vacuum-dried to obtain Situmage 1000 (145.17g...

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Abstract

The invention provides a preparation method of cetomacrogol 1000, characterized by comprising the steps of (1) dissolving polyethylene glycol a dry organic solvent, adding metallic sodium under stirring and nitrogen protection, and heating to allow refluxing reaction; (2) cooling, dropwise adding bromohexadecane, and heating to allow refluxing reaction to obtain cetomacrogol 1000. The method allows cetomacrogol to be prepared only under the normal pressure by heating and refluxing; the method has no need for high pressure equipment, is simple and safe to perform, and prevents the defects thatethylene oxide is flammable and explosible and carcinogenic and requires strict transport conditions; the method has the advantages that the materials are simple and easy to attain, the process is simple and good in safety, equipment input cost is low, no geographic restrictions occur, and the method is applicable to large-range large-scale production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of Situmage 1000. Background technique [0002] Cetomacrogol 1000 (Cetomacrogol-1000), also known as polycetol 1000 or cetyl polyoxyethylene ether, ceteth-20, is often used as an emulsifier for emulsions and creams, and a solubilizer for volatile oils. The CAS number is 9004-95-9, and the structural formula of Citumago is as formula (I). [0003] [0004] Cetomago 1000 is currently mainly produced by the reaction of cetyl alcohol or stearyl alcohol with ethylene oxide. Currently, Cetomaco 1000 on the market adopts the industrial classic method: using potassium cetyl alcohol and ethylene oxide in 18-crown Under the catalysis of ether-6, react under high temperature and high pressure (140°C, 70psi), and then undergo purification treatment to obtain Situmage 1000. The synthetic route is as follows: [0005] [0006] Most domestic enterprises adopt the a...

Claims

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Application Information

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IPC IPC(8): C08G65/338C08G65/337
CPCC08G65/337C08G65/338
Inventor 冯汝华黄铁强黄晓健杨溢贝荣丙黄锦坚曾国超
Owner 汕头经济特区鮀滨制药厂
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