921-88-0Relevant academic research and scientific papers
Synthesis process of difluoroacetic acid
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Paragraph 0022; 0025; 0028; 0031; 0034; 0037; 0041, (2021/11/14)
The synthesis process comprises the following steps: adding dialkylamines in a dry reaction vessel, first organic solvent and volume concentration of 10 - 40% alkali liquor, dropwise adding dichloroacetyl chloride, carrying out heat preservation stirring after dropwise addition, organic subtraction pressure desolventizing and concentrating to obtain dichloroacetyl dialkylamine. Potassium fluoride, second organic solvent and dichloroacetyl dialkylamine were added to another reaction vessel, and the molar ratio @timetime@ and thermal insulation of the potassium fluoride, the solvent diethylene glycol and the dichloroacetyl 3:5:1 dialkylamine is @. The equimolar difluoroacetyl dialkylamine and the volume concentration were mixed with 10 - 30% lye, reflux was 4 - 10h, dichloroacetyl dialkylamine was recovered by distillation, and the bottoms of the bottoms were adjusted pH=1 with hydrochloric acid and distilled again to give difluoro acetic acid.
Method for preparing ethyl bromodifluoroacetate
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Paragraph 0025, (2018/04/02)
The invention provides a method for preparing ethyl bromodifluoroacetate and relates to a preparation method of a chemical reagent. The method takes trichloro ethylene as a raw material, and comprisesthe following steps: under the action of ultraviolet light of a catalytic medium, an oxidation reaction happens between trichloro ethylene and oxygen in a reactor to synthesize dichloracetyl chloride; an amination reaction happens between dichloracetyl chloride and diethylamine under the action of a catalyst to synthesize dichloroacetyl diethylamine; a fluorination reaction happens between dichloroacetyl diethylamine and anhydrous potassium fluoride under the action of a solvent and a phase transfer catalyst to synthesize difluoroacetyl diethylacetamide; difluoroacetyl diethylacetamide is esterified to synthesize ethyl difluoroacetate; and by taking cupric bromide as a brominating agent, ethyl difluoroacetate is bromized to prepare the end product (ethyl bromodifluoroacetate). The methodhas the characteristics that the equipment investment is low, reaction conditions are mild, the method is safely implemented at normal pressure, and after-treatment is simple.
Sequential reactions promoted by manganese: Completely stereoselective synthesis of (E)-α,β-unsaturated amides, ketones, aldehydes, and carboxylic acids
Concellon, Jose M.,Rodriguez-Solla, Humberto,Diaz, Pamela
, p. 7974 - 7979 (2008/02/13)
(Chemical Equation Presented) A complete E-selective synthesis of α,β-unsaturated amides through a sequential reaction of a range of dichloroamides with a variety of aldehydes promoted by Rieke manganese (Mn*) is reported. A mechanism based on a sequential aldol-type reaction and a completely stereoselective β-elimination is proposed to explain these results. The unsaturated amides obtained are readily and efficiently transformed into α,β-unsaturated ketones, aldehydes, or carboxylic acids without loss of the diastereoisomeric purity of the C-C double bond.
Transformations of N-ethylamines into amide derivatives under the action of sulfur monochloride
Konstantinova,Berezin,Rakitin
, p. 1178 - 1183 (2008/09/19)
Tertiary N-ethylamines were converted into amide derivatives by reactions with sulfur monochloride and DABCO at 0 °C. Depending on the nature of the substituents in the amine, the reaction can be accompanied by unexpected transformations.
Direct conversion of N-ethylamines into functionalised amides by S2Cl2
Konstantinova,Rakitin,Rees
, p. 167 - 168 (2007/10/03)
Hünig's base 1 is known to react extensively with S2Cl2 to give monocyclic, bicyclic and fused tricyclic 1,2-dithioles with the N-ethyl group intact, but with S2Cl2 and DABCO in chloroform at 0 °C 1 is converted
Enantioselective Oxidation of Thioethers: Synthesis of trans-2-N,N-Dialkylacetamide-1,3-dithiolanes-S-oxide and Their Use in Asymmetric Aldol-Type Reactions
Corich, Martina,Furia, Fulvio Di,Licini, Giulia,Modena, Giorgio
, p. 3043 - 3044 (2007/10/02)
(-)-trans-2-N,N-dialkylacetamide-1,3-dithiolanes-S-oxide 2 have been obtained in high d.e. (>99:1) and e.e.(up to 94percent, >98percent after crystallization) by enantioselective oxidation .The aldol-type addition of the magnesium enolate of the N,N-diethyl derivative (-)-2b to iso-butyraldehyde afforded good chemical yields of a single diastereomer.Key Words: Enantioselective oxidation; Asymmetric aldol-type addition, trans-(-)-2-N,N-Diethylacetamide-1,3-dithiolane-S-oxide.
SYNTHESIS OF DICHLOROKETENE ACETALS UNDER CONDITIONS OF PHASE-TRANSFER CATALYSIS AND THEIR REACTIONS WITH SULFUR-CONTAINING ELECTROPHILES
Guseva, S. A.,Mirskova, A. N.,Levkovskaya, G. G.,Kalikhman, I. D.,Voronkov, M. G.
, p. 261 - 268 (2007/10/02)
A method was developed for the production of dichloroketene acetals by the dehydrochlorination of chloral acetals in DMFA in the presence of triethylbenzylammonium chloride as phase-transfer catalyst.Sulfur monochloride, sulfur dichloride, and benzene sulfenyl chloride react with dichloroketene acetals with the formation of adducts (alkoxycarbonyldichloromethanesulfenyl chloride ClSCCl2COOR, alkoxycarbonyldichloromethanethiosulfenyl chloride ClSSCCl2COOR, and butyl phenylthiodichloroacetate C6H5SCCl2COOR respectively).The action of secondary amines on butoxycarbonyldichloromethanesulfenyl chloride gave sulfenamides R1R2NSCCl2COOBu.The reactions of butoxycarbonyldichloromethanethiosulfenyl chloride and butyl phenylthiodichloroacetate with secondary amines under various conditions led to degradation products.
REACTIVITY OF CHLOROSUBSTITUTED α-EPOXIDES AND SYNTHESES UNDER THESE COMPOUNDS
Voronina, T. A.,Fomina, N. V.,Suminov, S. I.
, p. 1059 - 1063 (2007/10/02)
The reactivity of chloroepoxyethanes in reactions with nucleophiles and electrophiles increases sharply with the accumulation of chlorine atoms on the epoxide ring.The reaction rate correlates with the nucleophile strength.Reactions with strong nucleophiles proceed through epoxide isomerization and lead to chloroacetic acid derivatives.Addition to the epoxide ring is found only for several weak nucleophiles.
