Method for producing liquid composition containing monoetherate, liquid composition, and method for producing polymerizable compound
A technology for polymerizable compounds and manufacturing methods, which is applied in the preparation of organic compounds, dehydration of hydroxyl-containing compounds to prepare ethers, organic chemical methods, etc.
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preparation example Construction
[0130] As hydroxides of alkali metals used in the preparation of the cleaning aqueous solution, etc., include: hydroxides of alkali metals such as sodium hydroxide and potassium hydroxide; hydroxides of alkaline earth metals such as calcium hydroxide; trisodium phosphate, Phosphates of alkali metals such as tripotassium phosphate; phosphates of alkaline earth metals such as calcium phosphate, etc.
[0131] Among these, from the viewpoint of obtaining the effects of the present invention more easily, alkali metal hydroxides or alkali metal phosphates are preferred, sodium hydroxide, potassium hydroxide, tripotassium phosphate are more preferred, sodium hydroxide, hydrogen Potassium oxide.
[0132] The amount of alkali metal hydroxide or the like used is not particularly limited, and the mole number of the hydroquinone compound (I) used in excess relative to the hydroxyl group-containing etherifying agent (II) (from the hydroquinone compound ( The number of moles of I) minus th...
Embodiment
[0206] Hereinafter, the present invention will be described in further detail based on examples. In addition, this invention is not limited to a following Example.
[0207] In the following examples and comparative examples, the compositions of the solution compositions were analyzed by high performance liquid chromatography.
[0208] At this time, the molar percentages of the hydroquinone compound (I), the monoether compound (III), and the diether compound (IV) were calculated by preparing calibration curves using high-purity standard substances.
[0209] In addition, in the following examples, the purity of 6-[(4-hydroxyphenyl)oxy]hexyl acrylate was calculated|required from the ratio of the peak area based on the high-speed liquid chromatography analysis.
[0210]
[0211] The measurement conditions of the high performance liquid chromatography are as follows.
[0212] Device: Agilent Corporation, 1200 series
[0213] Eluent: a mixture of acetonitrile (liquid A) and 0.1...
Synthetic example 1
[0219] (Synthesis example 1) Liquid composition analysis of the organic phase after step (1)
[0220] In a 3-port reactor with a cooler and a thermometer, in a nitrogen stream, add 104.77g (0.9515mol) of hydroquinone, 100g (0.7320mol) of 6-chlorohexanol, 500g of distilled water, and 100g of benzene methyl ether. While stirring all the contents, 35.13 g (0.8784 mol) of sodium hydroxide was further added. When adding, the temperature of the contents was added in small amounts over 20 minutes so that the temperature of the contents would not exceed 40°C. After completion of the addition of sodium hydroxide, the contents were heated and reacted under reflux conditions (99° C.) for 10 hours.
[0221] After completion of the reaction, the temperature of the reaction solution was lowered to 60° C., and after standing for 10 minutes, the aqueous phase was removed by liquid separation. The residual organic phase was analyzed by high performance liquid chromatography.
[0222] As a r...
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Abstract
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