53626-93-0Relevant articles and documents
Process for preparing ketazine by molecular oxygen oxidation method
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Paragraph 0052-0055, (2019/07/04)
The invention discloses a process for preparing ketazine by a molecular oxygen oxidation method, which comprises the following steps: ketimine is prepared, and ketone and ammonia are put into a pressure kettle according to a ratio;a pressure range is adjusted to be1.0-5.0MPa, a temperature range to be30-180 DEG C, and a reaction time to be 3-5 hours to generate the ketimine; the molar ratio of theammonia to the ketone is 1:1-20:1; the temperature and the pressure are reduced, and a mixture of the ketimine and the ketone is separated; the mixture of the ketimine and the ketone, a catalyst anda drying agent are put into a reaction kettle and heated to 30-80 DEG C, molecular oxygen is introduced to perform oxidation reaction, wherein the pressure range is 0-1.0MPa, and the reaction time is3-6 hours, and molecular oxygen included: oxygen or air; ketazine is separated and purified.The method is not only suitable for benzophenone, but also achieves theketazine of aliphatic ketone with fewcarbon atoms. The method has wide source of raw materials, low cost and easy recovery, no saline wastewater, low energy consumption and cost, and is environmentally friendly.
Molecular structure of 2-butanimine, an unstable imine, as studied by gas electron diffraction combined with MP2 and DFT calculations
Egawa,Konaka
, p. 2085 - 2090 (2007/10/03)
The molecular structure of 2-butanimine (C(4)H3-C(3)H2-C(2)(-C(5)H3)=N(1)H) was determined by means of gas electron diffraction. The sample of 2-butanimine, an unstable imine, was prepared by vacuum gas-solid reaction of N,N-dichloro-2-butanamine ((C2H5)(CH3)CH-NCl2) and KOH in a glass column. The column temperature and sample pressure were optimized by measuring FTIR spectra of the reaction products in a separate experiment. The results of MP2 and DFT calculations were used as supporting information. The coexistence of the (E)-sp and (E)-ac conformers was assumed. The structural parameters (rg and ∠α) obtained for the (E)-sp conformer are as follows: r(C=N) = 1.285(3) A; 〈r(C-C)〉 = 1.514(2) A; 〈r(C-H)〉 = 1.113(3) A; r(N-H) = 1.046 A (dependent); ∠N=-C-C(3) = 115.8(5)°; ∠N=C-C(5) = 125.0(5)°; ∠C-C-C(4) = 115.2(12)°; ∠C-C(4)-H = 113.5(14)°; ∠C=N-H = 109.3 (assumed). Angle brackets denote averaged values, and parenthesized values are the estimated limits of error (3σ) referring to the last significant digit. The dihedral angle, φNCCC, of the (E)-ac conformer was assumed to be 117.6°. The abundance of the (E)-sp conformer was determined to be 60 ± 10% at room temperature.
REACTIONS RETRODIENIQUES-IX. SYNTHESE PAR THERMOLYSE ECLAIR ET ETUDE D'ENAMINES PRIMAIRES INSTABLES
Ripoll, J. L.,Lebrun, H.,Thuillier, A.
, p. 2497 - 2504 (2007/10/02)
Etheneamine 1 and its methyl derivatives 2-7 have been synthesized from the adducts 8-14 by a retro-Diels-Alder reaction under flash thermolytic conditions.The primary enamines 1-4 have been identified (IR, (1)H and (13)C NMR in a pure state at -80 deg C; at the same temperature, the enamines 5-7, less stable, are already accompanied by their tautomeric imines 33 or 34.When warmed up to room temperature, the enamines 1-7 lead, following to their substitution, either to nitrogen heterocycles (30, 42) or to acyclic azadienes (35-37, 39, 40).
