5458-14-0Relevant academic research and scientific papers
METHOD FOR PRODUCING IMIDAZOLINE COMPOUND
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Paragraph 0036; 0040, (2021/06/04)
PROBLEM TO BE SOLVED: To provide a method for producing an imidazoline compound having high yield and small amount of impurity. SOLUTION: There is provided a method for producing an imidazoline compound (B) using a diamine monoamide compound (A) represented by the general formula (1), wherein the method includes a dehydration condensation step of the diamine monoamide compound (A) and a distillation step of the imidazoline compound (B). In the dehydration condensation step, the temperature of the dehydration condensation reaction of (A) is 100°C to 160°C in a time of 50% or more of the process time from when the conversion rate from (A) to (B) becomes 55% until when the conversion rate from (A) to (B) becomes 70%, and a the gas-phase pressure at the temperature of the dehydration condensation reaction of (A) is P1 which satisfies the conditions 1. In the distillation step, the temperature of the liquid containing (A) and (B) is 100°C to 190°C in a time of 50% or more of the process time from when 30 wt.% of the total distillate of (B) is distillated until when 90 wt.% of the total distillate of (B) is distillated, and a pressure (B) in the gas-phase of the distillation step is P2 which satisfies the condition 2. SELECTED DRAWING: None COPYRIGHT: (C)2021,JPOandINPIT
Green synthesis method of sitagliptin intermediate
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Paragraph 0032; 0037-0039; 0047-0048; 0052-0053, (2021/10/27)
The invention relates to a green synthesis method of sitagliptin intermediate, and belongs to the technical field of drug intermediate synthesis. In order to solve the problems that an existing pollution is large and unstable, a green synthesis method of sitagliptin intermediate is provided, and the method comprises the following steps: in an ether solvent, reacting trifluoroacetic acid ethyl ester with ethylenediamine to generate 2 - trifluoroacetamide ethyl ethylamine. Under the presence of an acid binding agent, 2 - trifluoroacetamide ethyl ethylamine and halogenated ethyl acetate are condensed and reacted under the conditions of 45 °C - 65 °C DEG C to form an intermediate, and then, the temperature is raised to 90 - 110 °C for cyclization reaction to generate N - trifluoroacetyl piperidine. The N -trifluoroacetyl piperidine ketone is reacted with hydrazine hydrate to generate 1 -trifluoroacetylamino -2 -piperazinone. The product is reacted with hydrochloric acid to form a ring-forming reaction, and a product sitagliptin intermediate is obtained. The method provided by the invention has the advantages of high product yield and purity on the whole, and has the advantage of environmental friendliness.
Multifunctional degradable nanoparticles with control over size and functionalities
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Page/Page column 141, (2018/02/03)
In one aspect, the invention relates to polymers, crosslinked polymers, functionalized polymers, nanoparticles, and functionalized nanoparticles and methods of making and using same. In one aspect, the invention relates to degradable polymers and degradable nanoparticles. In one aspect, the invention relates to methods of preparing degradable nanoparticles and, more specifically, methods of controlling particle size during the preparation of degradable nanoparticles. In one aspect, the degradable nanoparticles are useful for complexing, delivering, and releasing payloads, including pharmaceutically active payloads. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present invention.
DENDRITIC MOLECULAR INTRACELLULAR TRANSPORTERS AND METHODS OF MAKING AND USING SAME
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Page/Page column 106, (2010/11/30)
In accordance with the purpose(s) of the invention, as embodied and broadly described herein, the invention, in one aspect, relates to compounds comprising the structure: and at least one guanidinium residue, wherein m is zero or a positive integer. Also disclosed are methods of preparing the disclosed compounds. Also disclosed are methods of intracellular delivery comprising administering the disclosed compounds and compositions to a subject. Also disclosed are pharmaceutical compositions comprising a therapeutically effective amount of one or more compounds or compositions of the invention and a pharmaceutically acceptable carrier. This abstract is intended as a scanning tool for purposes of searching in the particular art and is not intended to be limiting of the present invention.
High yield selective acylation of polyamines: Proton as protecting group
Oganesyan, Asmik,Cruz, Iris A.,Amador, Roberto B.,Sorto, Nohemy A.,Lozano, Jose,Godinez, Carlos E.,Anguiano, Jaime,Pace, Heather,Sabih, Ghiwa,Gutierrez, Carlos G.
, p. 4967 - 4970 (2008/03/28)
An advance in the selective acylation of polyamines having identical or similar amine functions is reported. While nucleophilicity differences between the various amine functions are slight, the corresponding conjugate acids exhibit pKa values
Ethyl trifluoroacetate: A powerful reagent for differentiating amino groups
Xu, Daqiang,Prasad, Kapa,Repic, Oljan,Blacklock, Thomas J.
, p. 7357 - 7360 (2007/10/02)
Selective protection of primary amines in the presence of secondary amines and monofunctionalization of symmetric primary and secondary diamines using ethyl trifluoroacetate is described. Effective differentiation of primary, secondary and tertiary alkyl-substituted primary amines from one another by ethyl trifluoroacetate acylation is also demonstrated. These results are explained on the basis of steric and electronic effects of the substrate amines.
