CN103787847A - Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent - Google Patents
Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent Download PDFInfo
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- CN103787847A CN103787847A CN201410047965.6A CN201410047965A CN103787847A CN 103787847 A CN103787847 A CN 103787847A CN 201410047965 A CN201410047965 A CN 201410047965A CN 103787847 A CN103787847 A CN 103787847A
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- 239000002904 solvent Substances 0.000 title claims abstract description 31
- HDPNBNXLBDFELL-UHFFFAOYSA-N 1,1,1-trimethoxyethane Chemical compound COC(C)(OC)OC HDPNBNXLBDFELL-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 17
- 238000005516 engineering process Methods 0.000 title description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 48
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 42
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 10
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 6
- -1 trifluoromethane sulfimide ion Chemical class 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 claims 1
- 150000001450 anions Chemical class 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- GBLIGNUYGOFIKS-UHFFFAOYSA-N 4-[2-(3,5-dioxopiperazin-1-yl)ethyl]piperazine-2,6-dione Chemical compound C1C(=O)NC(=O)CN1CCN1CC(=O)NC(=O)C1 GBLIGNUYGOFIKS-UHFFFAOYSA-N 0.000 description 6
- DNMZJIGSDQVGSA-UHFFFAOYSA-N methoxymethane;hydrochloride Chemical compound Cl.COC DNMZJIGSDQVGSA-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003905 agrochemical Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- YMRPKBLFDBUOAJ-UHFFFAOYSA-N 5-butyl-2-methyl-1h-imidazole Chemical group CCCCC1=CN=C(C)N1 YMRPKBLFDBUOAJ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002470 thermal conductor Substances 0.000 description 1
- 150000005199 trimethylbenzenes Chemical class 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/60—Preparation of compounds having groups or groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C257/00—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines
- C07C257/04—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines without replacement of the other oxygen atom of the carboxyl group, e.g. imino-ethers
- C07C257/06—Compounds containing carboxyl groups, the doubly-bound oxygen atom of a carboxyl group being replaced by a doubly-bound nitrogen atom, this nitrogen atom not being further bound to an oxygen atom, e.g. imino-ethers, amidines without replacement of the other oxygen atom of the carboxyl group, e.g. imino-ethers having carbon atoms of imino-carboxyl groups bound to hydrogen atoms, to acyclic carbon atoms, or to carbon atoms of rings other than six-membered aromatic rings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for preparing trimethyl orthoacetate by using hydrophobic ionic liquid as a solvent. The method comprises the following steps: feeding anhydrous acetonitrile, anhydrous methanol and the solvent into a reaction kettle, cooling to -5 DEG C, feeding dry hydrogen chloride gas into the kettle, afterwards, stirring and reacting for 6 hours, wherein the solvent is the hydrophobic ionic liquid; feeding mixed liquid into a second reaction kettle, adding precooled methanol at the temperature of 5 DEG C, stirring for 0.5 hour, adjusting the pH value of a reaction system to 5-6 by using ammonia gas, and carrying out alcoholysis on the mixed liquid for 12 hours at the temperature of 40 DEG C; cooling alcoholysis liquid to 0 DEG C, adjusting pH value to 8.0 by using ammonia gas, feeding the alcoholysis liquid into an ordinary pressure rectifying tower, and collecting 107-109 DEG C fractions so as to obtain the trimethyl orthoacetate; and feeding residue at the bottom of the rectifying tower into a washing kettle, washing, feeding lower liquid into a drying kettle, drying, and recycling the dried solvent. The method has the advantages that the cost is saved, the energy consumption is reduced, and the green production of the trimethyl orthoacetate is realized.
Description
Technical field
The present invention relates to a class hydrophobic ionic liquid and prepare the method for trimethyl orthoacetate as solvent.
Background technology
Trimethyl orthoacetate (CAS:11445-45-0) is a kind of colourless transparent liquid, is soluble in the organic solvent such as alcohol, ether, except for New Sweetening Agent Trichlocromethyl Sucrose synthetic, is widely used in the chemical such as medicine, agricultural chemicals, spices.Trimethyl orthoacetate synthetic method bibliographical information both domestic and external is few, mainly contains sodium Metal 99.5 method and acetonitrile method, and wherein with acetonitrile method report at most, this method raw material is easy to get, is widely used.
According to relevant report, in industrial production, generally use low boiling point solvent, as anhydrous diethyl ether, sherwood oil, chloroform, tetracol phenixin, benzene, toluene, (the Peter P.T.Sah such as ethanol, J.Am.Chem.Soc., 1928, 50:516, S.M.McElvain, J.Am.Chem.Soc., 1942, 64:1825, analogy reason moral, In Jiangxi Science, 2005, 23 (6): 744, Yu Mingxing, agricultural chemicals, 1991, 30 (5): 19, sand is gone away for some great undertakings, Anhui chemical industry, 1992, (2): 11, Lin Yuehua, Guangdong chemical industry, 1999, (5): 26, Lu Xueliang, application chemical industry, 2003, 32 (2): 21, Li Jing, Guangzhou chemistry, 1992, (2): 61).Owing to can producing ethyliminum methyl ether hydrochloride, chloride solid precipitation in producing, need to add the low boiling point solvent of 5-6 times of volume to disperse.Aftertreatment is cumbersome, need to first steam solvent, then steam product.Not only energy consumption is high for this method, solvent loss is large, and product heated time is long, is prone to decomposition, causes yield not high.
In recent years, there is bibliographical information to adopt high boiling solvent, as (Chen Kun, agricultural chemicals such as kerosene, chlorobenzene, dibutyl phthalate, trimethylbenzenes, 2004,43 (11): 507, Zhou Xueyong, Yunnan chemical, 2000,27 (5): 4), product is in the time separating, and solvent can be used as thermal conductor, only need to steam trimethyl orthoacetate.Although this method has been simplified technique, before distillation, byproduct ammonium chloride still needs suction filtration to separate, and solvent needs again to purify after repeatedly recycling, and its wastage rate also can be up to 27%.
Summary of the invention
The object of the invention is to adopt a class hydrophobic ionic liquid to prepare trimethyl orthoacetate as solvent, for the building-up process of trimethyl orthoacetate, this class ionic liquid has following feature: can dissolve intermediate ethyliminum methyl ether hydrochloride and by-product ammonium chloride, thereby make technological process be easy to realize complete canalization operation, can recycle ionic liquid by washing, can recycled for multiple times and substantially there is no loss, thus realize the simplification of technique and improve product yield.
One class hydrophobic ionic liquid is prepared the method for trimethyl orthoacetate as solvent, its flow process is shown in accompanying drawing 1, and it comprises the following steps:
In formula: R
1be selected from the straight chained alkyl of C4～C8;
The mixed solution that step 2. obtains step 1 is conveyed in the second reactor (E-2), temperature in the kettle is 5 ℃, add the pre-cold methanol of two times of anhydrous acetonitrile molar weights and stir 0.5h, the pH value that regulates reaction system with ammonia in liquid ammonia storage tank (E-3) to pH be 5-6, then at 40 ℃ of left and right alcoholysis mixed solution 12h;
The step 3. alcoholysis liquid to 0 ℃ that cooling step 2 obtains in the second reactor (E-2), by ammonia adjusting pH value to 8.0, afterwards alcoholysis liquid is conveyed into atmospheric distillation tower (E-4), collects 107～109 ℃ of cuts, obtain product trimethyl orthoacetate;
At the bottom of step 4. rectifying tower (E-4) tower, still liquid is sent in washing kettle (E-5) and is washed, and lower floor's liquid is sent in drying kettle (E-6) and dried, and the solvent after oven dry is sent in the first reactor (E-1), carries out recycle.
Invention before the present invention is better than: the method is by being used hydrophobic ionic liquid as solvent, solubilized intermediate ethyliminum methyl ether hydrochloride and solid by-product ammonium chloride, thereby make technological process be easy to realize complete canalization operation, be conducive to realize the serialization of technique, distillation is before without suction filtration operation.Meanwhile, the still liquid after distillation finishes, can remove through simple washing the ammonium chloride by product being dissolved in ionic liquid, and ionic liquid can recycle after drying, and provides cost savings and has reduced energy consumption, has realized the green production of trimethyl orthoacetate.
Accompanying drawing explanation
Fig. 1 is that the present invention uses hydrophobic ionic liquid to prepare the process flow diagram of trimethyl orthoacetate for solvent, wherein: E-1 is the first reactor; E-2 is the second reactor; E-3 is liquid ammonia storage tank; E-4 is rectifying tower; E-5 is washing kettle; E-6 is drying kettle.
Embodiment
Embodiment 1: adopt butyl methyl imidazoles hexafluorophosphate as solvent
In reactor, drop into anhydrous acetonitrile 41.0g(1mol), anhydrous methanol 32.0g(1mol) and butyl methyl imidazoles hexafluorophosphate 73.0g, reaction solution is stirred and is cooled to-5 ℃, slowly pass into dry hydrogen chloride gas 36.5g(1mol by distribution pipe), after logical finishing, slowly temperature is risen to 5 ℃, simultaneously abundant stirring reaction 6h, obtains ethyliminum methyl ether hydrochloride solution.Solution is cooled to 0 ℃, and adds wherein precooling anhydrous methanol 64.0g(2mol), with ammonia regulation system pH=5.5, temperature is risen to 40 ℃ and stirring reaction 12h.Cooling reaction solution to 0 ℃, with ammonia regulation system pH to 8.0.By reaction solution air distillation and collect 107 ℃～109 ℃ cuts, obtain trimethyl orthoacetate 110.76g, yield is 92.3%.
Be similar to embodiment 1, under different condition, operate, acquired results is as shown in the table:
| Embodiment | Solvent quality (g) | Alcoholysis pH value | Product yield % |
| 2 | 109.5 | 5.5 | 93.4 |
| 3 | 146.0 | 5.5 | 93.8 |
| 4 | 73.0 | 5.0 | 90.2 |
| 5 | 73.0 | 6.0 | 85.0 |
Note: solvent is butyl methyl imidazoles hexafluorophosphate
Embodiment 6:
In reactor, drop into anhydrous acetonitrile 41.0g(1mol), anhydrous methanol 32.0g(1mol) and hexyl methyl imidazoles hexafluorophosphate 73.0g, reaction solution is stirred and is cooled to-5 ℃, slowly pass into dry hydrogen chloride gas 36.5g(1mol by distribution pipe), after logical finishing, slowly temperature is risen to 5 ℃, simultaneously abundant stirring reaction 6h, obtains ethyliminum methyl ether hydrochloride solution.Solution is cooled to 0 ℃, and adds wherein precooling anhydrous methanol 64.0g(2mol), with ammonia regulation system pH=5.5, temperature is risen to 40 ℃ and stirring reaction 12h.Cooling reaction solution to 0 ℃, with ammonia regulation system pH to 8.0.By reaction solution air distillation and collect 107 ℃～109 ℃ fractions, obtain trimethyl orthoacetate 113.52g, yield is 94.6%.
Be similar to embodiment 6, adopt different ionic liquids to operate, acquired results is as shown in the table:
| Embodiment | Solvent | Product yield % |
| 7 | Octyl group Methylimidazole hexafluorophosphate | 95.8 |
| 8 | Butyl-pyridinium hexafluorophosphate | 92.6 |
Embodiment 9:
In reactor, drop into anhydrous acetonitrile 41.0g(1mol), anhydrous methanol 32.0g(1mol) and the octyl group Methylimidazole hexafluorophosphate 73.0g that reclaims of embodiment 7, reaction solution is stirred and is cooled to-5 ℃, slowly pass into dry hydrogen chloride gas 36.5g(1mol by distribution pipe), after logical finishing, slowly temperature is risen to 5 ℃, simultaneously abundant stirring reaction 6h, obtains ethyliminum methyl ether hydrochloride solution.Solution is cooled to 0 ℃, and adds wherein precooling anhydrous methanol 64.0g(2mol), with ammonia regulation system pH=5.5, temperature is risen to 40 ℃ and stirring reaction 12h.Cooling reaction solution to 0 ℃, with ammonia regulation system pH to 8.0.By reaction solution air distillation and collect 107 ℃～109 ℃ cuts, obtain trimethyl orthoacetate 114.12g, yield is 95.5%.
Be similar to embodiment 9, the octyl group Methylimidazole hexafluorophosphate that Reusability reclaims, acquired results is as shown in the table:
| Embodiment | Recycle number of times | Product yield % |
| 10 | 5 | 94.8 |
| 11 | 10 | 93.6 |
| 12 | 15 | 92.7 |
| 13 | 20 | 91.6 |
Claims (1)
1. a class hydrophobic ionic liquid is prepared the method for trimethyl orthoacetate as solvent, it is characterized in that comprising the following steps:
Step 1. is by anhydrous acetonitrile, anhydrous methanol and solvent are sent in the first reactor (E-1) and are carried out subcooling, the consumption of solvent is anhydrous acetonitrile and anhydrous methanol total mass 1-2 times, the consumption of anhydrous methanol and anhydrous acetonitrile equimolar amount, be cooled to temperature for-5 ℃ of left and right, to passing in still and the dry hydrogen chloride gas of anhydrous acetonitrile equimolar amount, afterwards fully about stirring reaction 6h, described solvent is a class hydrophobic ionic liquid, its positively charged ion is N, N-dialkylimidazolium positively charged ion or N-alkyl pyridine cationoid, negatively charged ion is the adjacent acid anion of hexafluoro or two trifluoromethane sulfimide ion, concrete chemical structural formula is:
In formula: R
1be selected from the straight chained alkyl of C4～C8;
The mixed solution that step 2. obtains step 1 is conveyed in the second reactor (E-2), temperature in the kettle is 5 ℃, add the pre-cold methanol of two times of anhydrous acetonitrile molar weights and stir 0.5h, the pH value that regulates reaction system with ammonia in liquid ammonia storage tank (E-3) to pH be 5-6, then at 40 ℃ of left and right alcoholysis mixed solution 12h;
The step 3. alcoholysis liquid to 0 ℃ that cooling step 2 obtains in the second reactor (E-2), by ammonia adjusting pH value to 8.0, afterwards alcoholysis liquid is conveyed into atmospheric distillation tower (E-4), collects 107～109 ℃ of cuts, obtain product trimethyl orthoacetate;
At the bottom of step 4. rectifying tower (E-4) tower, still liquid is sent in washing kettle (E-5) and is washed, and lower floor's liquid is sent in drying kettle (E-6) and dried, and the solvent after oven dry is sent in the first reactor (E-1), carries out recycle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072346A (en) * | 2014-06-19 | 2014-10-01 | 常州吉恩化工有限公司 | Method for preparing orthoester compound |
| CN111675607A (en) * | 2020-06-09 | 2020-09-18 | 杭州众立化工科技有限公司 | Method for producing trimethyl orthoacetate through differential circulation and continuous production |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060678A (en) * | 2010-12-27 | 2011-05-18 | 江苏优士化学有限公司 | Synthesis process of trimethyl orthoacetate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060678A (en) * | 2010-12-27 | 2011-05-18 | 江苏优士化学有限公司 | Synthesis process of trimethyl orthoacetate |
Non-Patent Citations (2)
| Title |
|---|
| ALEKSEI B. SHEREMETEV ET AL.,: "Synthesis of 2-R-2,2-dinitroethanol orthoesters in ionic liquids", 《MENDELEEV COMMUNICATIONS》, vol. 15, no. 5, 31 December 2005 (2005-12-31), pages 204 - 205, XP022533448, DOI: 10.1070/MC2005v015n05ABEH002157 * |
| SAITHALAVI ANAS ET AL.,: "Ionic Liquid [bmim]PF6-Mediated Synthesis of 1,2-Orthoesters", 《BULL. CHEM. SOC. JPN.》, vol. 80, no. 3, 31 December 2007 (2007-12-31), pages 553 - 560 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072346A (en) * | 2014-06-19 | 2014-10-01 | 常州吉恩化工有限公司 | Method for preparing orthoester compound |
| CN111675607A (en) * | 2020-06-09 | 2020-09-18 | 杭州众立化工科技有限公司 | Method for producing trimethyl orthoacetate through differential circulation and continuous production |
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