529-64-6Relevant articles and documents
Synthesis method of 3-hydroxy-2-phenylpropionic acid
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Paragraph 0024; 0027-0029; 0030; 0032-0035; 0036; 0039-0041, (2019/12/25)
The invention discloses a synthetic method of 3-hydroxyl-2-phenylpropionic acid. The method comprises the following steps: mixing dimethyl sulfoxide, paraformaldehyde, potassium carbonate powder and methyl phenylacetate, heating to 85-95 DEG C, carrying out gas phase monitoring reaction, and cooling to room temperature when the GC content of the product methyl tropine is more than or equal to 70%;adjusting the pH value to be neutral, and performing reduced pressure distillation for desolvation; then adding methanol into the desolventized mixture, dropwise adding a sodium hydroxide solution, and reacting to obtain a mixed solution containing sodium tropine salt; adjusting the pH value of the mixed solution to 2-3, and completely reacting to obtain a crude product; and finally, recrystallizing the crude product sequentially by using methylbenzene of which the ratio of m product to m methylbenzene is 1: (4-6), methylbenzene/water of which the ratio of m product to m methylbenzene to m water is 1: (1-2): (4-6), and water of which the ratio of m product to m water is 1: (4-6) to obtain a pure product of 3-hydroxyl-2-phenylpropionic acid. According to the method, GC is adopted to monitor the reaction, control points are judged quickly and accurately, purification of methyl tropinate is not needed, operation procedures are reduced, and production cost is reduced. According to the method, the purity of the prepared 3-hydroxyl-2-phenylpropionic acid reaches 99% or above while the yield is ensured to reach 76.5% or above.
Gold(I)/copper(II)-cocatalyzed tandem cyclization/semipinacol reaction: Construction of 6-Aza/Oxa-Spiro[4.5]decane skeletons and formal synthesis of (±)-halichlorine
Zhu, Dao-Yong,Zhang, Zhen,Mou, Xue-Qing,Tu, Yong-Qiang,Zhang, Fu-Min,Peng, Jin-Bao,Wang, Shao-Hua,Zhang, Shu-Yu
, p. 747 - 752 (2015/03/18)
A simple and efficient strategy for the construction of 6-aza/oxa-spiro[4.5]decane skeletons under the cocatalysis of gold(I)/copper(II) was developed, and its potential utility was demonstrated by a formal synthesis of the biologically active marine alkaloid (±)-halichlorine.
Selective reductions of cyclic 1,3-diesters using SmI2 and H2O
Guazzelli, Giuditta,Grazia, Sara De,Collins, Karl D.,Matsubara, Hiroshi,Spain, Malcolm,Procter, David J.
supporting information; experimental part, p. 7214 - 7215 (2009/10/16)
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