- Method for preparing aminoacetaldehyde dimethyl acetal
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The invention discloses a method for preparing aminoacetaldehyde dimethyl acetal, which comprises the following steps: S1, adding a phase transfer catalyst A and vinyl acetate into a reaction flask, introducing a certain amount of chlorine while stirring, and performing heat-insulation stirring until the color of the reaction solution becomes colorless to obtain a chlorination solution; S2, dropwise adding the chlorination liquid prepared in the step S1 into methanol for reaction to prepare a chloroacetaldehyde dimethyl acetal crude product; S3, transferring the chloroacetaldehyde dimethyl acetal crude product prepared in the step S2 to an autoclave, introducing liquid ammonia, carrying out heating and pressurizing reaction, and after the reaction is finished, adding alkali to adjust the pH value; and S4, decompressing and rectifying the reaction product to obtain the target product, aminoacetaldehyde dimethyl acetal. By adopting the method, high-purity aminoacetaldehyde dimethyl acetal can be prepared, and the industrial production requirement of aminoacetaldehyde dimethyl acetal can be met.
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Paragraph 0047; 0050; 0051; 0054; 0055; 0058
(2020/11/22)
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- Technology for producing aminoacetaldehyde dimethyl acetal
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The invention discloses a new technology for producing aminoacetaldehyde dimethyl acetal. Chloroacetaldehyde dimethyl acetal is firstly synthesized into aminoacetaldehyde dimethyl acetal by using ammonia solution containing carbon dioxide, aminoacetaldehyde dimethyl acetal and carbon dioxide are then converted to hydroxymethyl aminopropyl formic acid, aminoacetaldehyde dimethyl acetal is preventedfrom continuously reacting with chloroacetaldehyde dimethyl acetal to generate secondary and tertiary amine, after deamination, hydroxymethyl propylcarbamic acid is decomposed into aminoacetaldehydedimethyl acetal and carbon dioxide after high temperature and acid aqueous reflux. After recovering carbon dioxide, aminoacetaldehyde dimethyl acetal hydrochloride is obtained, and then aminoacetaldehyde dimethyl acetal hydrochloride is neutralized, distilled and rectified to obtain high purity aminoacetaldehyde dimethyl acetal.
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Paragraph 0014-0016
(2019/08/20)
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- Photorelease of primary aliphatic and aromatic amines by visible-light-induced electron transfer
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Visible-light-absorbing tris(bipyridyl)ruthenium(II) has been used to mediate electron transfer to N-methylpicolinium carbamates that undergo C-O bond fragmentation followed by spontaneous carbon dioxide release to give free amines. Release of several aliphatic and aromatic primary amines has been demonstrated under mild conditions using visible light.
- Edson, Joseph B.,Spencer, Liam P.,Boncella, James M.
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supporting information; experimental part
p. 6156 - 6159
(2012/01/05)
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- Synthesis of chiral primary amines: diastereoselective alkylation of N-[(1E)-alkylidene]-3,5-bis[(1S)-1-methoxyethyl]-4H-1,2,4-triazol-4-amin es and N4-Nexocyclic bond cleavage in the resulting 1,2,4-triazol-4-alkylamines
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Enantiomerically pure 3,5-bis[(1S)-1-methoxyethyl]-4H-1,2,4-triazol-4-amine 14a and 3,5-bis[(1S)-1-ethoxyethyl]-4H-1,2,4-triazol-4-amine 14b were used as chiral auxiliaries to obtain enantiomerically enriched α-aminoacetals, primary alkyl and arylalkyl amines (ee ranging from 40% to 90%). The different stages of the process were imine formation from the corresponding aldehydes, diastereoselective addition of a Grignard reagent, quaternization of the triazole auxiliary and cleavage of the N4-Nexocyclic bond by LiBH4. The mechanism of the cleavage of the N4-Nexocyclic bond is supported by the use of deuterated metal hydride. The absolute configurations of the new stereogenic centres were established by X-ray analyses of the enantiomerically pure stereomers isolated by semi-preparative liquid chromatography on a chiral support.
- Serradeil-Albalat, Muriel,Roussel, Christian,Vanthuyne, Nicolas,Vallejos, Jean-Claude,Wilhelm, Didier
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body text
p. 2682 - 2692
(2009/04/07)
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- Amine compounds, resist compositions and patterning process
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Amine compounds having a cyano group are useful in resist compositions for preventing a resist film from thinning and also for enhancing the resolution and focus margin of resist.
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- Functionalized derivatives of hyaluronic acid, formation of hydrogels in situ using same, and methods for making and using same
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Methods for chemical modification of hyaluronic acid, formation of amine or aldehyde functionalized hyaluronic acid, and the cross-linking thereof to form hydrogels are provided. Functionalized hyaluronic acid hydrogels of this invention can be polymerized in situ, are biodegradable, and can serve as a tissue adhesive, a tissue separator, a drug delivery system, a matrix for cell cultures, and a temporary scaffold for tissue regeneration.
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- SUBSTITUTED QUINAZOLINE DERIVATIVES AND THEIR USE AS INHIBITORS
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The use of a compound of formula (I) 1 or a salt, ester or amide thereof; where X is O, or S, S(O) or S(O)2, or NR6 where R6 is hydrogen or C1-6 alkyl,; R5 is an optionally substituted 5-membered heteroaromatic ring, R1, R2 ,R3, R4 are independently selected from various specified moieties, in the preparation of a medicament for use in the inhibition of aurora 2 kinase. Certain compounds are novel and these, together with pharmaceutical compositions containing them are also described and claimed
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- New and mild allyl carbamate deprotection method catalyzed by electrogenerated nickel complexes
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A Ni(II)-catalyzed electrochemical procedure for the simple and mild deprotection of allyl carbamates to the corresponding amines is described. The amines are obtained in yields of 40-99% and the method is compatible with several functional groups. Electrolyses are carried out in DMF or in THF in single-compartment cells in the presence of a consumable zinc anode. (C) 2000 Elsevier Science Ltd.
- Franco,Dunach
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p. 7333 - 7336
(2007/10/03)
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- Substituen Effect of Chelated Cobalt. 5. Acidities of (Carboxymethyl)- and (1-Carboxyethyl)cobaloximes. A Quantitative Analysis of the β Effect
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pKa's of the weakly acidic (carboxymethyl)(ligand)cobaloximes and (1-carboxyethyl)(ligand)cobaloximes with 16 different axial ligands have been determined and correlated with those of 11 substituted acetic acids or 9 1-substituted propionic acids, respectively.Comparison of apparent ?1 values thus calculated with those previously determined by correlation of (carboxyethyl)(ligand)cobaloxime pKa's with the pKa's of 2-substituted propionic acid indicates that the (1-carboxyalkyl)cobalt comlexes show a substantial β effect as an apparent extreme donation density to the carboxyl carbon.The β effect in these complexes has been quantitated by use of a dual substituent parameter equation, the results of which show that the effect is only some 8-10percent enhanced in (1-carboxyethyl)cobaloximes relative to (carboxymethyl)cobaloximes.This result is consistent with the β effect being mediated by ?-? hyperconjugation rather than neighboring group participation.Structural effects on the extent of ?-? conjugation and the effects of ?-? conjugation on reactivity of the cobalt atom in these complexes are discussed.
- Brown, Kenneth L.,Zahonyi-Budo, Eva
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p. 4117 - 4124
(2007/10/02)
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- Method of preparing aminoacetaldehyde acetals by the hydrogenation of dialkoxyacetonitrile
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A process for the preparation of an aminoacetaldehyde acetal of the formula STR1 wherein R is a saturated branched or unbranched alkyl radical of 1 to 4 carbon atomms By contacting a dialkoxyacetonitrile of the formula STR2 wherein R has the same meaning with hydrogen at an elevated pressure and at a temperature of 50-180° C., preferably in the presence of a catalyst and preferably in the presence of ammonia.
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