2680-03-7Relevant articles and documents
Formation of N, N-Dimethylacrylamide by a Multicenter Hydrocarbamoylation of C2H2 with N, N-Dimethylformamide Activated by Ru5(μ5-C)(CO)15
Adams, Richard D.,Tedder, Jonathan D.
, p. 5707 - 5710 (2018)
Hydrocarbamoylation of C2H2 by N,N-dimethylformamide (DMF) to N,N-dimethylacrylamide was effected by a series of cluster-opening reactions with Ru5(μ5-C)(CO)15 (1). The reaction of 1 with DMF yielded the new complexes Ru5(μ5-C)(CO)14(μ-n2-O=CNMe2)(μ-H) (2) and a minor coproduct Ru5(μ5-C)(CO)13(HNMe2)(μ-n2-O=CNMe2)(μ-H) (3) by a cluster-opening activation of the formyl C-H bond of DMF. Compound 3 was obtained from 2 by a further reaction with DMF. Compound 3 reacted with C2H2 (1 atm, 70 °C) to yield Ru5(μ5-C)(CO)13(μ-n3-O=CNMe2CHCH)(μ-H) (4) by the addition and coupling of C2H2 to the bridging dimethylformamido ligand. Compound 4 contains a σ-π-coordinated, dimethylformamido-substituted vinyl ligand that bridges a Ru-Ru edge of an open Ru5C cluster. The formamido group is also coordinated to one of the metal atoms. The addition of CO (1 atm, 25 °C) to 4 yielded the CO adduct Ru5(μ5-C)(CO)14(n2-O=CNMe2CH=CH)(μ-H) (5) containing a chelating dimethylacrylamido ligand, which released dimethylacrylamide by the reductive elimination of a C-H bond upon a further addition of CO (400 psi, 125 °C) with the re-formation of 1. All of the products were characterized by single-crystal X-ray diffraction analyses.
Amide bond formation in aqueous solution: Direct coupling of metal carboxylate salts with ammonium salts at room temperature
Nielsen, John,Tung, Truong Thanh
supporting information, p. 10073 - 10080 (2021/12/10)
Herein, we report a green, expeditious, and practically simple protocol for direct coupling of carboxylate salts and ammonium salts under ACN/H2O conditions at room temperature without the addition of tertiary amine bases. The water-soluble coupling reagent EDC·HCl is a key component in the reaction. The reaction runs smoothly with unsubstituted/substituted ammonium salts and provides a clean product without column chromatography. Our reaction tolerates both carboxylate (which are unstable in other forms) and amine salts (which are unstable/volatile when present in free form). We believe that the reported method could be used as an alternative and suitable method at the laboratory and industrial scales. This journal is
Palladium-catalyzed regioselective synthesis of B(4,5)-or B(4)-substituted: O-carboranes containing α,β-unsaturated carbonyls
Li, Jiaoyi,Lu, Jian,Tian, Song,Wang, Qian,Zhang, Chuyi,Zhang, Jianwei,Zhou, Ling
supporting information, p. 4723 - 4727 (2020/07/13)
With the help of a carboxylic acid directing group, Pd-catalyzed regioselective synthesis of B(4,5)-or B(4)-substituted o-carboranes containing α,β-unsaturated carbonyls has been reported. The-COOH, removed during the course of the reaction, is responsible for controlling the regioselectivity. The desired products could be obtained in moderate to good yields.
PRODUCTION METHOD OF N,N-DISUBSTITUTED α,β-UNSATURATED CARBOXYLIC ACID AMIDE AND CATALYST FOR PRODUCTION OF N,N-DISUBSTITUTED α,β-UNSATURATED CARBOXYLIC ACID AMIDE
-
Paragraph 0070-0101, (2020/03/31)
To provide a production method capable of producing N,N-disubstituted α,β-unsaturated carboxylic acid amide by a gas phase reaction.SOLUTION: The production method is a method for producing N,N-disubstituted α,β-unsaturated carboxylic acid amide by subjecting N,N-disubstituted carboxylic acid amide and aldehydes to a gas phase reaction in the presence of a catalyst. The catalyst includes an oxide of a first metal element being a metal element of Group 2 of the Periodic Table and an oxide of a second metal element being at least one kind of metal element selected from the group consisting of Mn, Cr, Co, Ni and Zn and has a mole ratio of the second metal element to the total mole number of the first metal element and the second metal element of 0.01 to 0.20.SELECTED DRAWING: None
N, N - disubstituted α, β - unsaturated carboxylic acid amide of (by machine translation)
-
Paragraph 0051; 0052; 0055; 0056; 0065; 0066, (2019/06/07)
[Problem] to compounds derived from compounds containing chlorine atoms contained in the byproducts of the no possibility, stable compound to N, N - disubstituted α, β - unsaturated carboxylic acid amide manufacturing method. [Solution] N, N - di-substituted carboxylic acid amide phenols with formaldehyde, in the presence of a catalyst containing no chlorine atoms, in a nonaqueous liquid phase reaction, N, N - disubstituted α, β - unsaturated carboxylic acid amide having a process, wherein the formaldehyde, paraformaldehyde, trioxane is one selected from formaldehyde and anhydrous 1, 3, 5 - 1, and the catalyst, an acidic catalyst or a basic catalyst N, α N - disubstituted, with production of β - unsaturated carboxylic acid amide. [Drawing] no (by machine translation)
Clickable coupling of carboxylic acids and amines at room temperature mediated by SO2F2: A significant breakthrough for the construction of amides and peptide linkages
Wang, Shi-Meng,Zhao, Chuang,Zhang, Xu,Qin, Hua-Li
, p. 4087 - 4101 (2019/04/30)
The construction of amide bonds and peptide linkages is one of the most fundamental transformations in all life processes and organic synthesis. The synthesis of structurally ubiquitous amide motifs is essential in the assembly of numerous important molecules such as peptides, proteins, alkaloids, pharmaceutical agents, polymers, ligands and agrochemicals. A method of SO2F2-mediated direct clickable coupling of carboxylic acids with amines was developed for the synthesis of a broad scope of amides in a simple, mild, highly efficient, robust and practical manner (>110 examples, >90% yields in most cases). The direct click reactions of acids and amines on a gram scale are also demonstrated using an extremely easy work-up and purification process of washing with 1 M aqueous HCl to provide the desired amides in greater than 99% purity and excellent yields.
N, N - disubstituted α, β - unsaturated carboxylic acid amide of (by machine translation)
-
Paragraph 0057; 0058, (2019/03/07)
The present invention is [a], the reaction time is short, suitable for mass-production by gas phase reaction N, N - disubstituted α, β - unsaturated carboxylic acid amide manufacturing method. [Solution] N, N - disubstituted α, β - unsaturated carboxylic acid amide is produced, N, N - disubstituted aldehyde carboxylic amide, in the presence of a catalyst, vapor phase reaction, N, N - disubstituted α, β - unsaturated carboxylic acid amide with. [Drawing] no (by machine translation)
MANUFACTURING METHOD OF β-SUBSTITUTED PROPIONIC ACID AMIDE AND N-SUBSTITUTED (METH)ACRYLAMIDE
-
Paragraph 0055; 0057; 0060; 0064, (2018/07/03)
PROBLEM TO BE SOLVED: To provide a method for industrially manufacturing β-alkoxy propionic acid amide, β-amino propionic acid amide and N-substituted (meth)acryl amide using (meth)acrylic acid ester as starting material at high yield and high purity. SOLUTION: There is provided a method for obtaining N-substituted (meth)acryl amide represented by target compound formula (7) by conducting an amidation reaction with amine using β-substituted propionic acid ester represented by the formula (1) of a product of a Michael addition reaction of (meth)acrylic acid ester and alcohol or amine in presence of a metal complex as a catalyst to obtain β-substituted propionic acid amide represented by the formula (3) and conducting a thermal decomposition reaction of β-substituted propionic acid amide in presence of the metal complex as the catalyst to eliminate alcohol or amine. A-CH2-C(R1)H-C(=O)-OR2 (1), A-CH2-C(R1)H-C(=O)-N(R3)R4 (3), CH2=C(R1)-C(=O)-N(R3)R4 (7) SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
RESORCINOL DERIVATIVE AS HSP90 INHIBITOR
-
Paragraph 0130, (2017/12/27)
The present invention relates to a compound represented by formula (I) of a resorcinol derivative as an HSP90 inhibitor or pharmaceutically accepted salts thereof. The compound in the present invention has the activity of inhibiting heat shock protein HSP90. Therefore, the compound in the present invention is used to treat proliferative diseases such as cancer and neurodegenerative diseases. The present invention further provides the compounds and preparation methods for pharmaceutical compositions comprising the compounds, a method for treating diseases, and pharmaceutical compositions comprising the compounds.
Method for synthesizing N,N-methacrylamide
-
Paragraph 0040; 0041, (2016/10/08)
The invention discloses a method for synthesizing N,N-dimethacrylamide. An acetylene-substituted complex and dimethylamino formyl halide are used as raw materials for synthesizing the N,N- dimethyl propiolamide. On the condition of a specific catalyzer, the N,N- dimethyl propiolamide and hydrogen are subjected to a reaction to generate the N,N-dimethacrylamide. According to the method for synthesizing the N,N-dimethacrylamide, alkynyl is introduced, the reliability of the preparation process is ensured, the product yield reaches 91.3% or above, and the purity is 95.6% or above. According to the synthesizing method, the reaction temperature is low, few side reactions are produced, the yield is high, the purity is high, and the method has the application prospect.
