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[ CAS No. 129188-99-4 ] {[proInfo.proName]}

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Chemical Structure| 129188-99-4
Chemical Structure| 129188-99-4
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Product Details of [ 129188-99-4 ]

CAS No. :129188-99-4 MDL No. :MFCD28167155
Formula : C21H26O2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W :310.43 Pubchem ID :-
Synonyms :

Safety of [ 129188-99-4 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P305+P351+P338 UN#:N/A
Hazard Statements:H315-H319-H335 Packing Group:N/A
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Application In Synthesis of [ 129188-99-4 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 129188-99-4 ]

[ 129188-99-4 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 873-94-9 ]
  • [ 108-95-2 ]
  • [ 129188-99-4 ]
YieldReaction ConditionsOperation in experiment
92.9% Stage #1: dihydroisophorone; phenol With phosphoric acid; water In water at 20℃; Heating / reflux; Stage #2: dihydroisophorone; phenol With sodium thiomethoxide at 20 - 40℃; for 9h; 1 EXAMPLE 1 [00029] 112.8 g (1.2 mol) of phenol, 16.9 g of water, 0.5 g of 75% aqueous solution of phosphoric acid and 7.2 g of BPTMCP crystals were placed in a one liter capacity four-necked flask provided with a thermometer, a dropping funnel, a reflux condenser and a stirrer to prepare a slurry. The slurry was adjusted at a temperature of 20° C. After the inside the flask was replaced by nitrogen gas, hydrogen chloride gas was introduced into the flask under stirring. The gas composition in the reaction vessel was analyzed and the volume concentration of hydrogen chloride gas was adjusted at 80%. [00030] 4.2 g of 15% aqueous solution of sodium methyl mercaptide was added dropwise to the slurry while the slurry was maintained at a temperature of 20° C., and then a mixture of 112.8 g (1.2 mol) of phenol and 42.0 g (0.3 mol) of TMC was added dropwise to the slurry over a period of six hours. The reaction mixture was found to increase in temperature during the addition, and when the addition was completed, the temperature was found to be 40° C. Then, the reaction was further continued at a temperature of 40° C. for anther three hours under stirring until completion. The reaction mixture was found to be slurry throughout the reaction from the start of the reaction when the mixture of phenol and TMC was added dropwise to the slurry to the completion of the reaction [00031] The resulting reaction mixture was analyzed by liquid chromatography. The production yield (mol of BPTMC produced/mol of starting TMC used) was found 92.9%.
92.9% With hydrogenchloride; phosphoric acid; sodium thiomethoxide In water at 20 - 40℃; for 9h; 1-5; 1 Example 1 A thermometer, a dropping funnel,Into a 1 L capacity four-necked flask equipped with a reflux condenser and a stirrer, 112.8 g (1.2 mol) of phenol,16.9 g of water, 0.5 g of 75% phosphoric acid and 7.2 g of BPTMC crystal were charged to obtain a slurry. The temperature was set to 20 ° C.,Under stirring,After replacing the interior of the reaction vessel with nitrogen gas, hydrogen chloride gas was introduced into the reaction vessel. The gas composition in the reaction vessel was analyzed and the volume concentration of hydrogen chloride gas was adjusted to 75%.While maintaining the temperature of the slurry at 20 ° C., 4.2 g of a 15% aqueous solution of methyl mercaptan sodium salt was added dropwise to the reaction vessel,Subsequently, a mixture of 112.8 g (1.2 mol) of phenol and 42.0 g (0.3 mol) of TMC was added dropwise over 6 hours, the temperature of the reaction mixture gradually increased, and at the end of the addition, it was 40 ° C. It was. After this, the reaction was further carried out for 3 hours to complete the reaction. The reaction mixture was in a slurry state from the beginning of the dropwise addition of the phenol and TMC mixture to the end of the reaction. Analysis of the reaction mixture thus obtained by liquid chromatography revealed that the aimed yield of BPTMC existence (molar amount of BPTMC produced / molar amount of raw material TMC) was 92.9%.
89.3 %Chromat. Stage #1: phenol With phosphoric acid In water at 20℃; Stage #2: With hydrogenchloride In water at 20℃; Stage #3: dihydroisophorone With sodium thiomethoxide In water at 20℃; for 6h; 1 Into a 1-L four necked flask equipped with a thermometer, a dropping funnel, a reflux condenser, and a stirrer were placed 188 g (2.0 moles) of phenol, 9.9 g of water, and 0.5 g of a 75% aqueous phosphoric acid solution, the temperature was adjusted to 20°C, and the air in the reaction system was replaced with nitrogen gas while stirring, after which hydrogen chloride gas was introduced. The gas component inside the reaction vessel was analyzed and the volumetric concentration of hydrogen chloride gas was adjusted to 80%. While maintaining the temperature at 20°C, 21 g of a 15% aqueous solution of methyl mercaptan sodium salt was added dropwise, and then a mixture of 188 g (2.0 moles) of phenol and 70.0 g (0.5 mole) of 3,3,5-trimethylcyclohexanone was added dropwise over a period of 3 hours. After completion of the addition dropwise, the reaction was continued for another 3 hours while maintaining the temperature at 20°C. After completion of the reaction, the resulting reaction mixture was identified using liquid chromatography and NMR analysis, which showed that the product was the BPTMC of interest and the yield (molar quantity of BPTMC produced/molar quantity of material TMC) was 89.3% (as measured by liquid chromatography). After completion of the reaction, the resulting reaction mixture was neutralized at pH 6.5 by adding an 18% aqueous sodium hydroxide solution while maintaining the temperature at 40-50°C. Next, the temperature of the reaction mixture thus neutralized was raised to 95°C to dissolve the generated BPTMC adduct crystals, after which the resulting water phase was removed by separation, and the temperature of the oil phase obtained was gradually lowered to 40°C with a temperature gradient of about 6°C/hour to crystallize the BPTMC-phenol adduct, and thus 177.9 g of crystals of the BPTMC-phenol adduct were obtained by centrifugal filtration. The result of liquid chromatography analysis showed that the adduct crystals thus obtained were consisted of 133.4 g of BPTMC, 44.2g of phenol and 0.3 g of remaining and had an APHA color value of 90 (10% methanol solution, as measured by the JIS method). Further, the trace impurities were 170 ppm sodium (as measured by atomic adsorption spectrometry) and 300 ppm sulfur (as measured by inductively coupled plasma atomic emission spectrometry).
62.5 %Chromat. With methanol; sulfuric acid; 1-dodecylthiol In toluene at 50℃; for 2.5h; Inert atmosphere; 33 Example 33 In a full-jacket type 1 L separable flask equipped with a thermometer, a stirrer, and a 100 mL dropping funnel, 5.0 g (0.2 mol) of methanol was added under a nitrogen atmosphere, and then 100 g (0.9 mol) of 92% by weight sulfuric acid was slowly added thereto to provide a solution in which monomethyl sulfate was produced. Thereafter, 54.3 g of toluene, 152 g (1.6 mol) of phenol, and 5.5 g (0.03 mol) of dodecanethiol were added thereto, followed by setting the temperature in the separable flask to 50° C. In the dropping funnel, 81 g (0.6 mol) of 3,3,5-trimethylcyclohexanone was added, and it was slowly fed dropwise to the separable flask for 30 minutes. After completion of the dropwise addition of 3,3,5-trimethylcyclohexanone, the reaction was allowed to proceed at 50° C. for 2 hours. After completion of the reaction, 100.0 g of ethyl acetate and 100.0 g of demineralized water were fed, and the resulting mixture was mixed. Thereafter, the mixture was left to stand, and the aqueous phase in the lower layer, was extracted. Thereafter, saturated sodium hydrogen carbonate solution was added to the obtained organic phase to allow neutralization, followed by confirming that the pH of the aqueous phase in the lower layer, became not less than 9. After extraction of the aqueous phase in the lower layer, demineralized water was added to the obtained organic phase, and the resulting mixture was stirred for 10 minutes. Thereafter, the mixture was left to stand, and the aqueous phase was extracted. Part of the obtained organic phase was removed, and subjected to measurement using a high-performance liquid chromatograph-mass spectrometer. As a result, a mass number of 309 (M+-1) was found in the negative mode, indicating production of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane. As a result of analysis using high-performance liquid chromatography, the production rate of 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane was found to be 62.5% by area
67 g With hydrogenchloride; mercaptoacetic acid In water at 25 - 30℃; 1; 1-5 Example 1 201.3 g of phenol, 50 g of 3,3,5-trimethylcyclohexanone, and 12.5 g of 3-mercaptopropionic acid were added to a 1000 ml reactor, and 50 g of 35% hydrogen chloride was slowly added to the reactor while maintaining the temperature at 25 to 30 ° C. After the reaction was progressed for 24 hours, the reaction was terminated and the pH of the reactant was adjusted to 7 to 7.5 by adding toluene and sodium hydroxide solution. Thereafter, the aqueous layer was removed by separation, and the reactants were washed with water. During the process of removing the water layer and washing with water, the pH of the reactant is adjusted to 8-8.5 by the remaining neutralized salt or aqueous alkali solution. The neutralized reactant, the pH of which was adjusted to 8 to 8.5, was heated and the temperature was adjusted to 60° C, and then 120 g of water and 3.26 g of a 23% sodium chlorite aqueous solution were added and sufficiently reacted, followed by separation to remove the aqueous layer. The input amount of sodium chlorite compared to the input amount of 3,3,5-trimethylcyclohexanone is 1.5% by weight. Since the input amount of 3,3,5-trimethylcyclohexanone is 50 g, the input amount of sodium chlorite is 1.5% by weight compared to the amount of 3,3,5-trimethylcyclohexanone input) The reactant from which the aqueous layer was removed was washed with water and then cooled to 40° C to precipitate crystals. The precipitated crystals were filtered and washed at room temperature using a mixture of phenol and toluene as a cleaning solvent. A mixture of phenol and toluene as a cleaning solvent was used as a mixture of phenol and toluene in a mass ratio of 7:3. After washing with a washing solvent was completed, the obtained product was re-dissolved in a mixture of water and toluene at 85 ° C. under normal pressure (mixing 1000% by weight of toluene with respect to water per unit mass), and then additionally washed with water and then heated to 40 ° C. By cooling, crystals were secondarily precipitated. Thereafter, the product was finally vacuum dried to obtain 67 g of 4,4'-(3,5,5-trimethyl cyclohexylidene)bisphenol.

  • 2
  • [ 27914-73-4 ]
  • [ 129188-99-4 ]
  • (3,3,5-trimethylcyclohexane-1,1-diyl)bis(1,4-phenylene)bis(4-acetoxybenzoate) [ No CAS ]
YieldReaction ConditionsOperation in experiment
89% With pyridine at 110℃; 1.2 (2) Preparation of (3,3,5-trimethylcyclohexane-1,1-diyl)bis(4,1-phenylene)bis(4-acetoxybenzoate) The commercial BPTMC 54g, 1 equiv. Available as diluted by stirring at room temperature, 159g of pyridine, 10 eq. After that Prior Synthesis of 4-acetoxy-benzoyl chloride 88.1g, 3 ~ 4 hours with stirring under reflux at 110 by the addition of 2.2 equivalent to slowly Respectively. Through the thin plate chromatography (TLC) the reaction was terminated by the addition of water after confirming the BPTMC are lost. Made to room temperature, ethyl acetate and 1N hydrochloric acid, and then extracted using distilled water, the organic layer over magnesium sulfate fractionation Removing the residual water remains in the organic layer, the organic layer was filtered to obtain the moisture removed. The organic layer obtained times Using the former evaporator under reduced pressure to remove the solvent. The solvent is removed substance was recrystallized using ethyl acetate and methanol, Of white solid of (3,3,5-trimethyl-cyclohexane-1,1-diyl) bis (4,1- phenylene) bis (4-acetoxy-benzoate).
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