590-93-2Relevant articles and documents
Thermal Stability of 2-Butynoic Acid (Tetrolic Acid)
Ashton, Hannah,Bethel, Paul A.,Cantlie, Sarah-Kate,Churchill, Trevor,Cooper, Katie,Dobson, Benjamin,Golden, Michael,Hoyle, Mark
, p. 1101 - 1104 (2019)
Work to assess the thermal properties of 2-butynoic acid (a precursor to acalabrutinib) has revealed the potential for thermal runaway on heating; testing using accelerated rate calorimetry (ARC) showed exothermic onset from 135 °C, precluding short-path distillation as a means of purification. Recrystallization was shown to be effective as an alternative technique to purify the compound and avoid the distillation procedure.
Rh-Catalyzed Asymmetric Hydrogenation of Unsaturated Medium-Ring NH Lactams: Highly Enantioselective Synthesis of N-Unprotected 2,3-Dihydro-1,5-benzothiazepinones
Yin, Congcong,Yang, Tao,Pan, Yingmin,Wen, Jialin,Zhang, Xumu
supporting information, p. 920 - 923 (2020/02/04)
A straightforward method to prepare 1,5-benzothiazepines was reported. Catalyzed by a Rh/Zhaophos complex, unsaturated cyclic NH lactams with a medium-size ring were hydrogenated smoothly, giving remarkably high enantioselectivities. The sulfur atom in the substrates did not bring an inhibition which was observed with commercially available bisphosphine ligands. This method was successfully applied in the scale-up synthesis of (R)-(-)-thiazesim.
Preparation method of 2-butynoic acid
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Paragraph 0050-0063, (2020/01/25)
The invention relates to the technical field of preparation of 2-butynoic acid, in particular to a preparation method of 2-butynoic acid. The preparation method provided by the invention comprises thefollowing steps: mixing 2-butyn-1-ol, a catalyst, hypochlorite, an alkaline substance and water, carrying out an oxidation reaction, and adding an acid to obtain the 2-butyne acid. On the basis of not using a phase transfer catalyst, high yield and purity of 2-butynoic acid are ensured. According to the embodiment, the high performance liquid chromatography (HPLC) purity of the 2-butynoic acid prepared by the preparation method is more than or equal to 99.6%, and the yield is more than or equal to 52.7%.