114059-99-3Relevant articles and documents
Hydroxylation of Alkyl Halides with Water in Ionic Liquid: Significantly Enhanced Nucleophilicity of Water
Kim, Dong Wook,Hong, Dong Jin,Seo, Jai Woong,Kim, Hoon Sik,Kim, Hong Kon,Song, Choong Eui,Chi, Dae Yoon
, p. 3186 - 3189 (2004)
A facile method for the nucleophilic hydroxylation of alkyl halides and mesylates with water has been developed in which the use of ionic liquid as an alternative reaction medium not only enhanced the nucleophilicity of water but also reduced the formation of elimination products predominantly formed under the conventional basic reaction conditions. For example, hydroxylation of model compound 2-(3-bromopropyl)naphthalene (1) to 2-(3-hydroxypropyl)-naphthalene (2) with water in 1-n-butyl-3-methylimidazolium tetrafluoroborate ([bmim] [BF 4]) and 1,4-dioxane proceeded selectively in high yield (94%). The reactivity of other nucleophilic oxygen sources such as alcohol, phenol, and acetic acid in an ionic liquid was also investigated.
Preparation method of bromhexine hydrochloride impurity C
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Paragraph 0036-0038; 0041-0043; 0046-0048; 0051-0053, (2020/08/25)
The invention relates to the field of chemical pharmacy, in particular to a preparation method of bromhexine hydrochloride impurity C: N-methyl-N-cyclohexyl-2-aminobenzene methylamine. The method hasobvious advantages in the aspects of rapidness, high efficiency and economy. The prepared high-purity N-methyl-N-cyclohexyl-2-aminobenzene methylamine has important significance for the quality research of bromhexine hydrochloride. The preparation method comprises the following steps: (1) adding o-aminobenzyl alcohol into thionyl chloride in batches, reacting at room temperature, evaporating a solvent to dryness after the reaction is finished, adding a pulping solvent, pulping and filtering to obtain a compound 1; (2) adding the compound 1 into N-methylcyclohexylamine in batches, reacting at room temperature, after the reaction is finished, adding a solvent, refluxing, decolorizing with activated carbon, filtering, and evaporating filtrate to dryness to obtain an impurity C.