74974-54-2Relevant articles and documents
Synthesis method of crude carboxylic ester (by machine translation)
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Paragraph 0021; 0022, (2020/08/09)
The method is characterized in that the carboxylic ester and the ether are prepared by reacting a carboxylic ester with an ether at a certain temperature under the catalysis of a catalyst at a certain pressure for a certain time. (by machine translation)
2-chlorine-1,1,1-trimethoxyethane preparing method
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Paragraph 0016; 0017, (2016/11/28)
The invention discloses a 2-chlorine-1,1,1- trimethoxyethane preparing method. The method is characterized by comprising the steps of 1, dissolving methyl chloroacetate in an organic solvent, lowering the temperature to -10-0 DEG C, and adding trimethyl orthoformate while stirring; 2, adding concentrated sulfuric acid solution with the mass concentration of 98% dropwise to the solution obtained from the step 1 at -10-0 DEG C; 3, heating the solution obtained from the step 2 to 30-80 DEG C for reaction for 1-3 h till reaction ends; 4, conducting vacuum concentration on the reaction liquid obtained in the step 3, adding the concentrated liquid to aqueous alkali, conducting extraction with ethyl acetate, washing the obtained ethyl acetate solution with saturated saline solution, conducting anhydrous sodium sulfate drying, and conducting vacuum concentration again to dry to obtain colorless oily liquid 2-chlorine-1,1,1- trimethoxyethane. According to the method, the reaction condition is mild, reaction time is short, production efficiency is high, cost is low, and the yield and purity of generated 2-chlorine-1,1,1- trimethoxyethane are quite high.
Divergent Diels-Alder methodology from methyl coumalate toward functionalized aromatics
Lee, Jennifer J.,Kraus, George A.
supporting information, p. 2366 - 2368 (2013/06/26)
An inverse electron-demand Diels-Alder reaction between methyl coumalate and electron-rich dienophiles produces substituted benzoates. A high-yielding, single-pot procedure transforms readily accessible vinyl ether, ketal, or orthoester dienophiles into functionalized aromatic systems in a versatile route.
Process for the production of 2-Chloro-1,1,1-trialkoxyethane
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Page 3, (2008/06/13)
Preparation of 2-chloro-1,1,1-trialkoxyethane involves reacting 1,1,1-trialkoxyethane with gaseous or liquid chlorine in the presence of alcohol solvent (0.1-20 wt.%) based on the amount of 1,1,1-trialkoxyethane reactant. Preparation of 2-chloro-1,1,1-trialkoxyethane of formula Cl-CH2-C(OR1)(OR2)(OR3) (I) involves reacting 1,1,1-trialkoxyethane with gaseous or liquid chlorine in the presence of alcohol solvent (preferably 1-10C) (0.1-20, preferably 5-20) wt.% based on the amount of 1,1,1-trialkoxyethane. R1-R3 = alkyl; R1+R2, R2+R3 and R1+R3 = a cyclic group.
A new synthesis of 1,2,4-triazolin-5-ones: Application to the convergent synthesis of an NK1 antagonist
Cowden,Wilson,Bishop,Cottrell,Davies,Dolling
, p. 8661 - 8664 (2007/10/03)
Chlorotriazolinone 4 has been synthesised in a single step via the novel condensation of semicarbazide hydrochloride with orthoester 8. Alkylation of secondary amine 3 with compound 4 proceeds in 99% yield to afford the target NK1 antagonist 1. (C) 2000 Published by Elsevier Science Ltd.
Synthesis of optically active 2-chloromethyl-2-oxazolines by the ortho- ester condensation method using triethyl orthochloroacetate
Kamata, Kazuyuki,Sato, Hideki,Takagi, Emi,Agata, Isao,Meyers
, p. 373 - 378 (2007/10/03)
A set of optically active 2-chloromethyl-2-oxazolines was synthesized by condensation of optically active 2-amino alcohols with triethyl orthochloroacetate which was prepared conveniently from triethyl orthoacetate by chlorination using tert-butyl hypochlorite.
NUCLEOPHILIC REACTIONS AT A VINYLIC CENTER. XXVIII. FLUOROCHLOROETHENES AND FLUOROBROMOETHENES IN REACTIONS WITH SODIUM ALCOHOLATES AND ARENETHIOLATES
Shainyan, B. A.,Vereshchagin, A. L.
, p. 1981 - 1988 (2007/10/02)
During the reaction of halogenoethenes (Z+E)-CHX=CFX with sodium methoxide and with sodium p-thiocresolate in methanol initial attack by the nucleophilic takes place at the carbon atom attached to the fluorine atom.In the reactions with sodium methoxide the intermediate monosubstitution products are more reactive than the initial halogenoethenes, and the main reaction products are the ortho esters CHXYC(OMe)3.An "element effect", i.e., concurrent substitution of F and Cl(Br) in the reaction with sodium methoxide, was discovered.With sodium p-thiocresolate trifluorochloroethene gives the product from substitution of the chlorine atom and a small amount of the addition product as impurity.The other ethenes give substitution, addition, and halogenophilic reduction products and also the products from further transformations (hydrolysis and decarboxylation).
Codeine Analogues. Synthesis of Spiro and Octahydro-1H-benzofuroisoquinolines
Moos, Walter H.,Gless, Richard D.,Rapoport, Henry
, p. 5064 - 5074 (2007/10/02)
A synthesis of highly functionalized spiro and octahydro-1H-benzofuroisoquinolines, analogues of codeine containing the benzofuran/piperidine and benzofuran/decahydroisoquinoline ring fragments, has been developed.The process extends to the dimethoxyphenyl series earlier work in the synthesis of 4a-aryldecahydroisoquinolines involving the α-methylene lactam rearrangement and utilizes a novel α-chloro ortho ester Claisen rearrangement to establish the requisite functionality for oxide ring closure.Selective ether cleavage is achieved with methanesulfonic acid/methionine to afford a spiro, and base-promoted rearrangement then yields the desired spiro.The C-ring is closed by Michael addition of a β-keto ester to the α-methylene lactam moiety, subsequently affording a protected benzofuroisoquinolone.Finally, amide reduction followed by ketone deprotection gives the desired cis- and trans-benzofuroisoquinolines.The entire synthesis can be performed by starting from o-vanillin with six purifications in 10percent overall yield, and the various intermediates additionally provide entries into the synthesis of 4-arylpiperidines, benzomorphans, and 4a-aryldecahydroisoquinolines.Functionality is built in to allow preparation of typical morphine patterns.
