4559-86-8Relevant articles and documents
Method for preparing tetrabutylurea by oil-water two-phase reaction system
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Paragraph 0015-0024, (2021/08/19)
The invention discloses a method for preparing tetrabutylurea by using an oil-water two-phase reaction system, which is characterized in that bis (trichloromethyl) carbonate and dibutylamine are used as raw materials, the oil-water two-phase reaction system is designed and provided, a solvent capable of effectively dissolving bis (trichloromethyl) carbonate and dibutylamine is adopted, meanwhile, a water phase is added into the reaction system to perform liquid seal on the reaction system, can absorb hydrogen chloride gas generated by the reaction at the same time, and promotes the forward proceeding of the whole reaction, and the method has the characteristics of high conversion rate, high selectivity and the like. The method for preparing tetrabutylurea by using the oil-water two-phase reaction system comprises the following steps: dissolving bis (trichloromethyl) carbonate in an organic solvent, placing the solution in a reactor, and simultaneously adding water into the reactor to perform liquid seal on the reaction system; and dissolving dibutylamine in an organic solvent, slowly injecting the dibutylamine into the organic solution of bis (trichloromethyl) carbonate through a micro-injection pump, carrying out chemical reaction, and carrying out refining treatment to obtain the product tetrabutylurea.
Method for preparation of 1, 1, 3, 3-tetrabutylurea by aqueous phase process
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Paragraph 0013; 0014; 0015; 0016; 0017; 0018; 0019-0022, (2017/03/08)
The invention discloses a method for preparation of 1, 1, 3, 3-tetrabutylurea by aqueous phase process. The method includes: adding bis(trichloromethyl)carbonate into a reaction container, and adding water; adding dibutylamine into the aqueous solution of bis(trichloromethyl)carbonate, and controlling the reaction temperature at 0-10DEG C; at the end of charging, further carrying out reaction for 1-9h; at the end of the reaction, separating the organic phase from the aqueous phase, conducting pickling and washing on the organic phase to remove impurities and a small amount of dibutylamine, and drying the organic phase to obtain 1, 1, 3, 3-tetrabutylurea; adding sodium hydroxide into the separated aqueous phase to conduct neutralization, and separating the organic phase to obtain dibutylamine, which can be directly used for reaction. The method takes water as the solvent, the reaction process is carried out at low temperature, and the method has the advantages of safety, environmental protection, low cost and strong operability.
Palladium-Catalyzed Oxidative N-Dealkylation/Carbonylation of Tertiary Amines with Alkynes to α,β-Alkynylamides
Mane, Rajendra S.,Bhanage, Bhalchandra M.
, p. 4974 - 4980 (2016/07/06)
The first highly effective Pd/C-catalyzed oxidative N-dealkylation/carbonylation of various aliphatic as well as cyclic tertiary amines with alkynes has been described. The selective sp3 C-N bond activation of tertiary amines at the less steric side using O2 as a sole oxidant and a plausible reaction pathway for the reaction are discussed. The general and operationally simple methodology provides an alternative for the synthesis of a wide range of alk-2-ynamide derivatives under mild conditions. The present protocol is ecofriendly and practical, and it shows significant recyclability.