18630-84-7Relevant academic research and scientific papers
Iridium-Catalyzed Unreactive C(sp3)-H Amination with 2,2,2-Trichloroethoxycarbonyl Azide
Zhang, Tao,Hu, Xuejiao,Dong, Xunqing,Li, Guigen,Lu, Hongjian
, p. 6260 - 6264 (2018)
An additive-assisted iridium-catalyzed directed C(sp3)-H amination with 2,2,2-trichloroethoxycarbonyl azide as an amino source is reported. Both carboxylate anions and the corresponding cations in the additives are crucial to achieve satisfactory efficiency. Sodium acetate or n-pentanoic acid can promote the amination of various primary C(sp3)-H bonds adjacent to secondary, tertiary, and quaternary carbons in ketoximes or N-aromatic heterocycles, respectively, providing a practical route to versatile β-amino ketoxime and N-heteroaryl ethanamine derivatives. The amination products can be treated as isocyanate analogues and can be converted to other useful amino functionalities. An iridacyclic compound was isolated and identified as a plausible intermediate.
Preparation method of benzyloxyamine hydrochloride
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Paragraph 0059-0063, (2021/04/14)
The invention discloses a preparation method of benzyloxyamine hydrochloride. The preparation method comprises the following steps: (1) dispersing ketoxime 2 and alkali metal hydroxide into a mixed solvent of dimethylacetamide and water at the temperature of 50-55 DEG C and the stirring speed of 100-120 rpm; (2) dropwise adding a benzyl halide compound 1 into a dispersion body obtained in the step (1), reacting for 130-140 minutes at the temperature of 60-65 DEG C after dropwise adding is completed, then cooling to room temperature, adding water, extracting by using normal hexane, and distilling an organic phase under reduced pressure to obtain a product 3; and (3) adding the product 3 obtained in the step (2) into a mixed solution of methanol and a hydrochloric acid solution with the mass concentration of 38% , reacting for 200-220 minutes at the temperature of 35-40 DEG C and at the stirring speed of 80-100 rpm, distilling under reduced pressure until a solid is separated out, cooling to room temperature, washing the solid with petroleum ether, and drying to obtain the target product 4-benzyloxyamine hydrochloride. According to the preparation method, the total yield can reach 95% or above, and the product purity can reach 99% or above.
