Structure of 13352-76-6
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The BI-3802 was designed by Boehringer Ingelheim and could be obtained free of charge through the Boehringer Ingelheim open innovation portal opnMe.com, associated with its negative control.
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CAS No. : | 13352-76-6 |
Formula : | C7H16O6 |
M.W : | 196.20 |
SMILES Code : | COCOCOCOCOCOC |
MDL No. : | MFCD26792351 |
Boiling Point : | No data available |
InChI Key : | VBVRQNRIUBCFDL-UHFFFAOYSA-N |
Pubchem ID : | 58099142 |
GHS Pictogram: |
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Signal Word: | Warning |
Hazard Statements: | H302-H315-H319-H335 |
Precautionary Statements: | P261-P305+P351+P338 |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With C16H36NO3S(1+)*CH3O4S(1-); at 125 - 130℃; under 26252.6 - 30003 Torr;Inert atmosphere; | To the reactor R1, the ionic liquid catalyst IL1 was added at a feeding speed of 9.8 g/h. When the catalystsolution began to circulate, the feeding was stopped, and the concentration of the catalyst was kept to be not less than4 wt.%. The initial feeding speeds of the concentrated formaldehyde and methanol were 170 mL/h and 68 mL/h, respectively.When the reaction materials began to circulate, the feeding speed of the formaldehyde was 70 mL/h. The operationconditions of the reactor R1 were controlled as 125?130C and 3.5?4.0 MPa. The reactor effluent liquid was fed intothe extraction tower C2. The feeding speed of the extraction agent, benzene, was 250 mL/h (being 1 fold more than thevolume of the reaction liquid). The heavy phase (the catalyst and aqueous formaldehyde solution) was continuously fedinto the film evaporator S2 from the tower bottom, where most of water was removed at 65C/-0.085 MPa, after that theheavy phase was fed into the reactor for reuse. The light phase (the product phase) was continuously fed into therectification tower C3 from the tower top. The light component, DMM1, methanol and formaldehyde, was continuously distilled from the tower top at 40?65C, and was fed back into the reaction unit for reuse, while the tower bottom liquidwas fed into the rectification tower C4. The extraction agent, benzene, distilled from the tower top at 78?80C was fedback into the storage tank V1 for reuse, while the tower bottom liquid was fed into the rectification tower C5. DMM2 andtrioxymethylene (the by-product) distilled from the tower top at 98?110C were fed back to the reaction unit for reuse,while the product, DMM3-8, flowing out from the tower bottom was fed into the product storage tank. Quantitative analysis of the samples taken from the reaction liquid, the extract, the aqueous catalyst solution,the recycled material and the product at certain interval was carried out by using the gas chromatograph. The test wasrun for 100 h totally. The average values of the test result were listed in Table 1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With C16H36NO3S(1+)*CH3O4S(1-); In water; at 125 - 130℃; under 26252.6 - 30003 Torr; | [0105] In the process shown in FIG. 1, the reactor R1 was a shell and tube reactor. The reactor R1 and the reactor heat exchanger were communicated with each other circularly, the reaction liquid was circulated in the reactor and the heat exchanger, and the volume was 500 mL. [0106] The air in the system was replaced by purging with high-purity nitrogen. To the formaldehyde concentrator S1, an aqueous formaldehyde solution having a concentration of 37 wt. % was continuously added at a feeding speed of 135 mL/h. The temperature of the concentrator S1 was controlled at 8090 C., and the vacuum degree thereof was controlled at -0.05-0.06 MPa. The vapor phase was fed into the dilute-aldehyde condenser E2 through the pipeline 3, and condensed to form liquid dilute formaldehyde, which was fed into the dilute-aldehyde receiving tank V3 through the pipeline 7 at a flow rate of 65 mL/h. The liquid phase was a formaldehyde solution of 60 wt. %, and delivered into the acetalization reactor R1 in C zone through the pipeline 5 at a flow rate of 70 mL/h. [0107] To the reactor R1, the ionic liquid catalyst IL1 was added at a feeding speed of 9.8 g/h. When the catalyst solution began to circulate, the feeding was stopped, and the concentration of the catalyst was kept to be not less than 4 wt. %. The initial feeding speeds of the concentrated formaldehyde and methanol were 170 mL/h and 68 mL/h, respectively. When the reaction materials began to circulate, the feeding speed of the formaldehyde was 70 mL/h. The operation conditions of the reactor R1 were controlled as 125130 C. and 3.54.0 MPa. The reactor effluent liquid was fed into the extraction tower C2. The feeding speed of the extraction agent, benzene, was 250 mL/h (being 1 fold more than the volume of the reaction liquid). The heavy phase (the catalyst and aqueous formaldehyde solution) was continuously fed into the film evaporator S2 from the tower bottom, where most of water was removed at 65 C./-0.085 MPa, after that the heavy phase was fed into the reactor for reuse. The light phase (the product phase) was continuously fed into the rectification tower C3 from the tower top. The light component, DMM1, methanol and formaldehyde, was continuously distilled from the tower top at 4065 C., and was fed back into the reaction unit for reuse, while the tower bottom liquid was fed into the rectification tower C4. The extraction agent, benzene, distilled from the tower top at 7880 C. was fed back into the storage tank V1 for reuse, while the tower bottom liquid was fed into the rectification tower C5. DMM2 and trioxymethylene (the by-product) distilled from the tower top at 98110 C. were fed back to the reaction unit for reuse, while the product, DMM3-8, flowing out from the tower bottom was fed into the product storage tank. [0108] Quantitative analysis of the samples taken from the reaction liquid, the extract, the aqueous catalyst solution, the recycled material and the product at certain interval was carried out by using the gas chromatograph. The test was run for 100 h totally. The average values of the test result were listed in Table 1. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With phosphoric acid; In water; at 80℃; for 4.0h; | To 250ml four-necked flask was added under mechanical stirring phenol (phenol and paraformaldehyde dimethyl ether molar ratio of 15:1), phosphoric acid (the molar ratio of phosphoric acid to paraformaldehyde dimethyl ether is 6.4: 1) and water (molar ratio of water and paraformaldehyde dimethyl etherRatio of 14: 1), the water bath was slowly heated to 80 C, and then 5 g of paraformaldehyde dimethyl ether was slowly added dropwise during the controlTemperature between 75 -85 C . Bi completed, maintaining the temperature at 80 C to continue the reaction 4h. Complete the reaction of raw materials, natural cooling to 45 C ,The reaction solution was poured into a separatory funnel, standing stratification, the lower phosphoric acid aqueous solution recovery applied. After the upper organic phase is neutralized by alkali,Concentrated under reduced pressure, the application of excess phenol recovery. The concentrate was diluted with ethyl acetate and washed successively with saturated aqueous ammonium chloride solutionWashed with water, dried over anhydrous sodium sulfate, suction filtered, the filtrate was concentrated to dry twice to obtain the crude product. Crude by high pressure liquid chromatographyMeasured, bisphenol F yield, selectivity and product distribution in Table 2. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42%Chromat.; 29%Chromat.; 14%Chromat. | With Amberlyst A15 resin; at 50℃; for 1.0h; | 100 g of methylal (also called dimethoxymethane CH3-OCH2-OCH3) (1.32 mol) and 30 g of trioxane (1 mol) were loaded into a 500 ml jacketed Schott reactor equipped with mechanical stirring, a condenser, and a temperature probe). 5 g of AmberlystR A15 resin, previously washed with methanol and dried under vacuum, are added. The mixture is heated to 50 C. and allowed to react for 1 hour. The reaction mixture is filtered and then washed with 10 g of 15% aqueous sodium hydroxide solution. The methylal is removed by evaporation under reduced pressure (90 C., 600 mBar (60,000 Pa) measured at the evaporator) on a rotary evaporator, then the POMM2 and the residual water are then removed by vacuum distillation. (Oldershaw type column with 10 trays) operating at a pressure of 200 mBar (20,000 Pa) at 90 C. 32 g of a cut POMM3-8 (CH3-(CH2O)n-OCH3 where n is 3 to 8) are obtained. (0061) The mass distribution of the product obtained is determined by GPC analysis as shown in Table 2. |
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