- A PROCESS FOR PREPARATION OF SULTONES
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The main object of present invention is to provide an economical and industrially applicable process for preparation of sultones of Formula (I). wherein n is 1-3 Sultones such as 1,3-propanesultone and 1,4-butanesultone are widely used as electroplating intermediates, pharmaceutical intermediates, photosensitive material, lithium batteries, and other household chemicals.
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Page/Page column 7-9
(2021/02/26)
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- Synthesis method of high-purity 1,4-butane sultone
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The invention discloses a synthesis method of high-purity 1,4-butane sultone. The synthesis method comprises the steps: 1, adding 4-chlorobutanol and a sodium sulfite solution into an alcohol solvent,raising the temperature until carrying out reflowing for 6 h, ending the reflowing to obtain a mixed solution A, concentrating the mixed solution A to recover the alcohol solvent, then, adding hydrochloric acid for acidification, carrying out concentration until a material becomes viscous, then, adding the alcohol solvent, separating out a sodium chloride crystal, carrying out filtration, and concentrating filtrate to recover the alcohol solvent so as to obtain 4-hydroxybutane sulfonic acid; 2, carrying out continuous flash evaporation dehydration on 4-hydroxybutane sulfonic acid at the vacuum degree of 1-8 mmHg and the temperature of 130-165 DEG C to obtain industrial-grade 1,4-butane sultone; and 3, adding an azeotrope into industrial-grade 1,4-butane sultone, carrying out normal-pressure fractional distillation to recover the azeotrope, then, carrying out reduced-pressure fractional distillation at the vacuum degree of 2-4 mmHg, and collecting fractions with the temperature of 120-121 DEG C to obtain high-purity 1,4-butane sultone. The method is simple and environment-friendly, the sulfonation yield is greatly increased, and the purity and yield of 1,4-butane sultone are greatly increased.
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Paragraph 0024-0033
(2019/02/13)
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- Preparation method of 1,4-butane sultone
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The invention relates to a preparation method of 1,4-butane sultone. The preparation method comprises the following steps: S1, putting 4-chlorobutanol and a sodium sulfite solution into a reaction vessel to be fully mixed, controlling the temperature to be 25-110 DEG C, performing reaction for 4-24h, and then, performing dehydration under reduced pressure for later use; S2, adding concentrated hydrochloric acid to the material subjected to dehydration under reduced pressure to perform acidification, controlling the temperature to be 25-100 DEG C and performing stirring for 1-12h, then performing cooling to room temperature, performing filtration, and concentrating the filtrate to obtain a concentrated solution containing 4-hydroxybutanesulfonate; S3, putting the concentrated solution in the vacuum environment to enable 4-hydroxybutanesulfonate to be subjected to dehydrated closed loop to obtain a crude product containing 1,4-butane sultone; and S4, performing rectifying treatment on the crude product obtained in the S3 to obtain 1,4-butane sultone. The preparation method provided by the invention has the beneficial effects that the process route is short, the dosages of acid and organic solvents are low, the post-treatment is simple, the total yield reaches 85% or above, and the purity of the product can reach 99.9% or above.
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Paragraph 0020; 0021; 0022
(2018/10/19)
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- 1,4-butane sultone and synthesis process thereof
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1,4-butane sultone and a synthesis process thereof relate to the field of fine chemical engineering. The synthesis process comprises the steps: performing sulfonation on 3-butylene-1-alcohol or 3-butylene-1-chlorine serving as a raw material and a sulfonating agent under the oxidation-reduction of an initiator; performing acidification after the reaction is finished; performing lactonization by high vacuum dehydration cyclization and azeotropic dehydration cyclization; and finally refining to obtain a 1,4-butane sultone finished product. The synthesis process of the 1,4-butane sultone, provided by the invention, is easily available in raw materials, few in synthesis steps, high in yield, high in product purity and suitable for industrialized production. The invention also provides the 1,4-butane sultone which is prepared by the synthesis process and has high purity.
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Paragraph 0050; 0056; 0062; 0067; 0073; 0078; 0084; 0095
(2017/07/23)
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- Monitoring of liquid-phase organic reactions by photoelectron spectroscopy
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There are strings attached: After linking the reacting groups to head groups of ionic liquids to drastically lower the vapour pressures of the reactants, ordinary liquid-phase organic reactions can be monitored by in situ X-ray photoelectron spectroscopy. This approach is demonstrated for the nucleophilic substitution of an alkyl amine and an alkyl chloride moiety, which are attached to the cation and anion of ionic liquids, respectively. Copyright
- Kolbeck, Claudia,Niedermaier, Inga,Taccardi, Nicola,Schulz, Peter S.,Maier, Florian,Wasserscheid, Peter,Steinrueck, Hans-Peter
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scheme or table
p. 2610 - 2613
(2012/04/17)
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- Chloroalkylsulfonate ionic liquids by ring opening of sultones with organic chloride salts
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An efficient route to prepare ionic liquids with chloroalkylsulfonate anions is presented; the synthesis proceeds in a one-step ring-opening reaction of sultones with an organic chloride salt and provides a very attractive access to new anion functionalised ionic liquids. The Royal Society of Chemistry.
- Paape, Natalia,Wei, Wei,Boesmann, Andreas,Kolbeck, Claudia,Maier, Florian,Steinrueck, Hans-Peter,Wasserscheid, Peter,Schulz, Peter Steffen
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body text
p. 3867 - 3869
(2009/02/07)
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- HYDROXYALKANESULFONYL CHLORIDES FROM CHLORINATION OF HYDROXYALKANESULFINATE SALTS IN A NONPOLAR MEDIUM: 3-HYDROXY-1-PROPANESULFONYL AND 4-HYDROXY-1-PROPANESULFONYL AND 4-HYDROXY-1-BUTANESULFONYL CHLORIDES
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3-Hydroxy-1-propanesulfonyl chloride (1b) was obtained for the first time (admixed with 10percent of propane sultone, 2b) by chlorination of a dichloromethane suspension of sodium 3-hydroxy-1-propanesulfinate 93b). 4-Hydroxy-1-butanesulfonyl chloride (1c) containing 13percent butane sultone (2c) was prepared similarly from 3c.The cyclizations of 1b and 1c in CDCl3 containing 1-butanol (0.9 M) showed first order rate constants of 1.4 x 10-4 and 6.4 x 10-5 s-1, corresponding to effective concentrations of 4.5 x 102 and 2.1 x 102 M, respectively.Reaction of triethylamine in ethanol-d (a) with 1b gave exclusively the undeuterated sultone (2b), evidently by a direct cyclization, and (b) with 1c produced mainly ethyl 4-hydroxy-1-butanesulfonate largely monodeuterated at the α-position, and presumably formed by way of the sulfene (6c).
- King, J. F.,Rathore, Rajendra
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p. 165 - 172
(2007/10/02)
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- ω-HYDROXY-1-ALKANESULFONYL CHLORIDES
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The general synthesis of hydroxyalkanesulfonyl chlorides is illustrated by the preparation of 6-hydroxy-1-butanesulfonyl cloride (2e) and 5-hydroxy-1-pentanesulfonyl chloride (2d) as fairly stable, only liquids (of ca. 95percent purity) charecterized by Hmr, Cmr and infrared spectra, and by conversion both to the corresponding sultones (3) and to crystalline acetoxy-piperidides (6); 2d and 2e form apparent polymers, very slowly on standing at room temperature and more rapidly on heating, but on reaction with triethylamine yield the sultones (3d and 3e).A sample consisting mostly (>70percent) of 4-hydroxy-1-butanesulfonyl chloride (2c), prepared and charecterized similarly, was found to form the sultone (3c) slowly in non-polar solvents, much more readily in polar media (t1/2 ca. 20 min in water), and very rapidly in the presence of triethylamine.Effective concentrations for the spontaneous cyclization of 4-hydroxy-1-butanesulfonyl chlorides (2c) and the tertiary-amine induced cyclizations of 2d and 2e are estimated at roughly 3x102, 0.1, and 0.05 M, respectively.The mechanism of the chlorination reaction and the origins of the different products with different substrates and reaction conditions are discussed.
- King, J. F.,Webster, Michael R.,Chiba, Naoki,Allen, Julie K.,Parker, Kenneth J. M.,et al.
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p. 161 - 176
(2007/10/02)
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