- Preparation method of amide compound
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The invention discloses a preparation method of an amide compound. The preparation method comprises the following steps: enabling a solution A containing a compound I to react with a solution B containing n-butyllithium at -80 to 10 DEG C, and then enabling a reaction solution to react with a solution C containing a compound II at -80 to 10 DEG C, wherein the concentration of the compound I in the solution A is 5 to 40 percent by weight, the concentration of the compound II in the solution C is 5 to 50 percent by weight, flow rates of the solution A and the solution C are respectively 0.1 to 25 L/s and 0.1 to 1.5 L/s, n is an integer of 0 to 5, and R1 is separately C1 to C6 alkyl, C1 to C6 alkoxy or substituted or un-substituted C6 to C10 aryl; R2 is hydrogen, C1 to C6 alkyl, or substituted or non-substituted phenyl, and a substituting group substituting the phenyl is C1 to C6 alkyl or C1 to C6 alkoxy; and R3 is C1 to C6 alkyl or one or more phenyl-substituted methyl.
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Paragraph 0069-0074
(2018/03/28)
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- A novel and efficient strategy for the synthesis of various carbamates using carbamoyl chlorides under solvent-free and grinding conditions using microwave irradiation
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We present an efficient, fast and simple strategy of generating the intermediate carbamoyl chlorides from secondary amines using stoichiometric amounts of bis(trichloromethyl)carbonate (BTC) in solution and solvent-free conditions with excellent yields. The results obtained showed the yield increasing on whether a base was used. Finally, an efficient and rapid synthesis of variety carbamate derivatives was developed by the reaction with a high variety of different alcohols, phenols, diols and this intermediate at room temperature with grinding and in solvent-free conditions under microwave irradiation. The presence of various safe bases is shown to be effective in reducing the reaction times, increasing the yields and easing purification. The present method does not involve any hazardous phosgene.
- Zare, Hassan,Ghanbari, Mohammad Mehdi,Jamali, Marzieh,Aboodi, Abdollah
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p. 883 - 886
(2012/08/28)
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- Ru-catalyzed hydrogenation of 3,5-diketo amides: Simultaneous control of chemo- and enantioselectivity
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By modulating the chelating priorities of the different directing groups in 3,5-diketo amides with the assistance from coordinating solvent, highly chemo- and enantioselective hydrogenation of the C3-carbonyls was achieved in the presence of [RuCl(benzene)(S)-SunPhos]Cl in THF.
- Li, Wanfang,Fan, Weizheng,Ma, Xin,Tao, Xiaoming,Li, Xiaoming,Xie, Xiaomin,Zhang, Zhaoguo
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supporting information
p. 8976 - 8978
(2012/11/07)
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- Facile N-arylation of amines and sulfonamides and O-arylation of phenols and arenecarboxylic acids
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An efficient, transition-metal-free procedure for the N-arylation of amines, sulfonamides, and carbamates and O-arylation of phenols and carboxylic acids has been achieved by allowing these substrates to react with a variety of o-silylaryl inflates in the presence of CsF. Good to excellent yields of arylated products are obtained under very mild reaction conditions. This chemistry readily tolerates a variety of functional groups.
- Liu, Zhijian,Larock, Richard C.
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p. 3198 - 3209
(2007/10/03)
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- Correlation of the rates of solvolysis of the N,N-diphenylcarbamoylpyridinium ion
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Solvolyses of the N,N-diphenylcarbamoylpyridinium ion are subject to specific and/or general base catalysis, which can be eliminated by addition of perchloric acid or increased, especially in fluoroalcohol-containing solvents, by addition of pyridine. The uncatalyzed solvolyses in aqueous methanol and aqueous ethanol involve a weakly nucleophilically assisted (l=0.22) heterolysis and the solvolyses in the pure alcohols are anomalously slow.
- Kevill, Dennis N.,Bond, Michael W.,D'Souza, Malcolm J.
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p. 273 - 276
(2007/10/03)
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- Kinetics and Selectivities for the Solvolysis of N,N-Diphenylcarbamoyl Chloride
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Values for the specific rates of solvolysis of N,N-diphenylcarbamoyl chloride have been analyzed using the two-term Grunwald-Winstein equation, incorporating the NT solvent nucleophilicity scale and the YCl solvent ionizing power scale.The sensitivities of 0.23+/-0.04 to changes in NT and of 0.58+/-0.03 to changes in YCl are consistent with an SN1 pathway with extensive internal nucleophilic assistance and a weak nucleophilic solvation of the developing carbocation.Product studies have been performed in mixtures of water with methanol, ethanol, and 2,2,2-trifluoroethanol (TFE) and in TFE-ethanol mixtures.Giving further support to the proposed SN1 mechanism, both the sensitivity to changes in solvent nucleophilicity and the product selectivities in aqueous ethanol and methanol parallel closely those previously determined for solvolyses of p-methoxybenzoyl chloride.
- D'Souza, Malcolm J.,Kevill, Dennis N.,Bentley, T. William,Devaney, Angela C.
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p. 1632 - 1637
(2007/10/02)
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- NOVEL SYNTHESES OF ARYLCARBAMIC ESTERS FROM CARBON DIOXIDE AND AROMATIC AMINE VIA A ZINC CARBAMATE.
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Arylcarbamic esters were synthesized directly from carbon dioxide and an aromatic amine via a zinc carbamate. The alkylation of the reaction mixture of carbon dioxide, an aromatic amine, and diethylzinc with dialkyl sulfate formed alkyl arylcarbamate in a high yield. Also, 2-hydroxycyclohexyl diphenylcarbamate was obtained selectively in a good yield by the reaction of carbon dioxide, epoxycyclohexane, and ethylzinc diphenylamide. Other arylcarbamates of 1,2-cyclohexanediol were obtained by the reactions of carbon dioxide, an aromatic amine, diethylzinc, and epoxycyclohexane.
- Yoshida,Ishii,Kawato,Yamashita,Yano,Inoue
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p. 2913 - 2916
(2007/10/02)
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- Reactions with Aziridines. XXIV: Amidoethylation of Esters of Monosubstituted Malonic Acids
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Diethyl phenylmalonate (1a) and methylmalonate (1b) have been amidoethylated with the N-acyl aziridines 3a-e under various conditions.In one case only (5) we were able to isolate the primarily formed amidoethyl derivative as minor product which otherwise cyclized apparently completely to form the corresponding N-acyl pyrrolidones 6a-f which mostly underwent further (alcoholytic) reactions.
- Budny, Jochen,Stamm, Helmut
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p. 657 - 664
(2007/10/02)
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