- Alkyl ether sulfonyl fluoride compound and synthesis method thereof
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The invention provides an alkyl ether sulfonyl fluoride compound and a synthesis method thereof. The method comprises the steps that an alkyl dihydric alcohol compound is taken as a start, firstly, sulfhydrylation is carried out so as to obtain a sulfhydryl compound containing monohydric alcohol; and the sulfhydryl compound reacts with halogenated alkane so as to obtain a sulfydryl-containing ether compound; the sulfydryl-containing ether compound is subjected to the action of thionyl chloride and alkali so as to obtain alkyl ether sodium sulfonate; and the alkyl ether sodium sulfonate is prepared into the alkyl ether sulfonyl fluoride compound under a fluorinating reagent. The alkyl ether sulfonyl fluoride compound can serve as a perfluoroalkyl substance precursor, and electrofluorinationis carried out so as to prepare a corresponding perfluoroalkyl substance. The alkyl ether sulfonyl fluoride compound has the advantages that different carbon chain numbers at the two ends of an etherchain compound can be provided, objective data can be provided for basic research, the compound can serve as a novel perfluoroalkyl ether compound precursor, a synthesis process is simple, raw materials are easy to obtain, and the method has relatively good atom economy and strong applicability.
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Paragraph 0043; 0044; 0045
(2019/01/08)
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- A 4 - mercapto -1 - butanol synthesis process
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The present invention discloses a 4-mercapto-1-butanol synthesis process, which comprises: 1) dissolving 1,4-butanediol and an acid-binding agent in an organic solvent I, adding a sulfonylation agent in a dropwise manner to carry out a sulfonylation reaction, carrying out extraction separation with dichloromethane, and carrying out washing, drying and concentration to obtain a colorless oil-like substance; and 2) dissolving the colorless oil-like substance obtained in the step 1) in an organic solvent II, adding a nucleophile to carry out a nucleophilic substitution reaction, and finally carrying out pressure reducing distillation to obtain the 4-mercapto-1-butanol. According to the present invention, the completely-new 4-mercapto-1-butanol synthesis route is provided, the used raw materials are easy to obtain, the operation is simple, the reaction conditions are not harsh, and good industrial values are provided.
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Paragraph 0035; 0036
(2017/05/02)
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- Sulfoboration of Cyclic Ethers - A Preparative Route to Mercaptoalkanols and Bis(hydroxyalkyl) Sulfides
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Bis(1,5-cyclooctanediylboryl) sulfide (1) reacts slowly with the cyclic ethers A-D to give O,S-bis(9-BBN)mercaptoalkanols 2a-d in excellent yields.From oxetane (E) and 1, however, 2e is obtained rapidly, which further reacts with E to yield the bis(9-BBN-oxypropyl) sulfide 3ee. 2a and c react with E to form the mixed thioethers 3ae and 3ce, respectively.The methanolysis of 2a-e leads to the O-(9-BBN)mercaptoalkanols 4a-e.The compounds 2 and 3 react with acetylacetone or with 2-aminoethanol to yield the mercaptoalkanols 7a-c, e and the bis(hydroxyalkyl) sulfides 8ae, 8ce and 8ee, resp., in high yields beside the 9-BBN-chelates 5 or 6.Key Words: Ethers, cyclic, cleavage of / Sulfoborations / Mercaptoethanols, 9-BBN derivatives of / Sulfides, bis(hydroxyalkyl), 9-BBN derivatives of
- Koester, Roland,Kucznierz, Ralf
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p. 835 - 842
(2007/10/02)
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- THE CHEMISTRY OF α,ω-MERCAPTOALCOHOLS IN THE PRESENCE OF DIETHOXYTRIPHENYLPHOSPHORANE. TEMEPERATURE DEPENDENCE OF CYCLODEHYDRATIONS AND S-ETHYLATIONS
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Diethoxytriphenylphosphorane (DTPP) is easily prepared by oxidative addition of triphenylphosphine with diethyl peroxide.DTPP converts a variety of mercaptoalcohols to cyclic sulfides as well as hydroxythioethers.The temperature dependence (+25 --> -25 deg C) of the product distribution has synthetic petential.
- Robinson, Philip L.,Kelly, Jeffery W.,Slayton, A. Evans
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- ACTIVITY OF 1-OXA-3-THIACYCLOALKANES AND 2-ALKYLTHIOOXACYCLANES IN FREE-RADICAL ISOMERIZATION
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It was established that radical isomerization to alkyl esters of thiocarboxylic acids, initiated by tert-butyl peroxide at 130-150 deg C, is a common reaction for five-, six- and seven-membered 1-oxa-3-thiacycloalkanes and 2-alkylthiooxacycloalkanes.Under analogous conditions 2-diethylaminotetrahydropyran isomerizes to N,N-diethylvaleramide.The relation between the structure and the reactivity of 1-oxa-3-thiacycloalkanes and 2-alkylthiooxacycloalkanes in free-radical isomerisation was studied by the method of competing reactions.Depending on the ring size, the activity of the 1-oxa-3-thiacycloalkanes increases in the order : 1,3-oxathianes 1,3-oxathiolanes 1,3-oxathiepanes.
- Zorin, V. V.,Batyrbaev, N. A.,Zlot-skii, S. S.,Rakhmankulov, D. L.
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p. 347 - 352
(2007/10/02)
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