33016-47-6Relevant articles and documents
Efficient molar-scale synthesis of 1-methyl-5-acylimidazole triflic acid salts
Chen, Bang-Chi,Skoumbourdis, Amanda P.,Sundeen, Joseph E.,Rovnyak, George C.,Traeger, Sarah C.
, p. 613 - 614 (2000)
A new process for the molar-scale preparation of 1-methyl-5-acylimidazole triflic acid salts was developed. The new process consists of: (i) regioselective 3N-tritylation of 5-acylimidazole to give 3-trityl-5-acylimidazoles, (ii) 1N-methylation of 3-trityl-5-acylimidazoles, and (iii) hydrolysis of the resulting quaternary ammonium salts to afford 1-methyl-5-acylimidazole triflic acid salts. This process is highly efficient, affording 1-methyl-5-acylimidazole triflic acid salts in 86-88% overall yield in three steps without chromatographic separation of products.
Expedient synthesis of N1-tritylimidazole-4-carboxaldehyde
Jetter, Michele C.,Boyd, Robert E.,Reitz, Allen B.
, p. 709 - 710 (1996)
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PURIFIED CRYSTALLINE DETOMIDINE HYDROCHLORIDE MONOHYDRATE, ANHYDRATE AND FREE BASE WITH LOW AMOUNTS OF ISO-DETOMIDINE AND OTHER IMPURITIES BY RECRYSTALLISATION IN WATER
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Page/Page column 26; 27, (2020/02/14)
The present disclosure relates to crystalline detomidine hydrochloride monohydrate, anhydrous detomidine hydrochloride and detomidine free base (4-[(2,3-dimethylphenyl)methyl]-1H-lmidazole ), purified by recrystallisation in water, with a low amount (total amount of impurities is not more than 0.1% area relative to detomidine based on HPLC, UV detection at 220 nm) of the impurities iso-detomidine (4-[(3,4-dimethylphenyl)methyl]-1H-lmidazole ), iso-impurity A (((RS)-(3,4-dimethylphenyl)(1H-imidazol-4-yl)methanol)), impurity A ((RS)-(2,3-dimethylphenyl)(1H-imidazol-4-yl)methanol), "ketone impurity" (2,3-dimethylphenyl)(1H-imidazol-4-yl) methanone, impurity B ((RS)-(1-benzyl-1H-imidazol-5-yl)(2, 3-dimethyl phenyl) methanol) and impurity C (4-[(2,3-dimethylcyclohexyl)methyl]-1H-imidazole). Also disclosed are processes for recrystallising detomidine hydrochloride monohydrate from commercially available anhydrous detomidine hydrochloride in water, pharmaceutical compositions comprising detomidine hydrochloride in purified form for use as an analgesic in methods of treating human subjects, a process for validating a batch of detomidine hydrochloride drug substance by determining the content of impurities iso-detomidine and iso- impurity A by HPLC, as well as XRPD, DSC and TGA data of crystalline detomidine free base.
Concise Synthesis of Anserine: Efficient Solvent Tuning in Asymmetric Hydrogenation Reaction
Yamashita, Megumi,Shimizu, Keita,Koizumi, Yasuaki,Wakimoto, Toshiyuki,Hamashima, Yoshitaka,Asakawa, Tomohiro,Inai, Makoto,Kan, Toshiyuki
supporting information, p. 2734 - 2736 (2016/11/30)
A concise synthesis of anserine and related compounds was accomplished by Et-DuPhos-Rh-catalyzed asymmetric hydrogenation of dehydrohistidine derivatives in 2,2,2-trifluoroethanol, which played a key role in improving the yield and selectivity.