- Preparation method of 4-ethoxy-1H-pyridine-2-ketone
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The invention discloses a preparation method of 4-ethoxy-1H-pyridine-2-ketone. The method comprises the following steps: dissolving 2,4-dichlorine-pyrimidine in solvent adding sodium ethoxide to reactto obtain 2-chlorine-4-ethoxy-pyrimidine; dissolving the 2-chlorine-4-ethoxy-pyrimidine in solvent and hydrolyzing to obtain the 4-ethoxy-1H-pyridine-2-ketone in alkaline condition. The preparation method of 4-ethoxy-1H-pyridine-2-ketone is simple, the raw material is easy to obtain, the product is easy to separate, the reaction condition is mild and easy to control, and the ketone is suitable for large-scale production. At that same time, chlorine gas, which is toxic gas, is not used in the two-step reaction, so that the environmental protection of the preparation is improved.
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Paragraph 0026; 0027
(2019/09/14)
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- Nucleosides and Nucleotides. 163. Synthesis of 3′-β-Branched Uridine Derivatives via Intramolecular Reformatsky-Type Reaction Promoted by Samarium Diiodide
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A novel efficient method for the synthesis of 3′-β-branched uridines starting from uridine was developed, in which a SmI2-promoted intramolecular Reformatsky-type reaction was effectively used. 5′-O-(Bromoacetyl)-3′-ketouridine derivatives 12, 26, and 27 were synthesized from uridine and were subjected to an intramolecular Reformatsky-type reaction. When 12, 26, and 27 were treated with 2.0 equiv of SmI2 in THF at -78°C, intramolecular carbon-carbon bond formation at the 3′-β-position proceeded smoothly to give the corresponding 3′,5′-lactones 14, 28, and 29 in high yields, respectively. Treatment of 28 with NH3/MeOH gave the 3′-β-branched uridine derivative 32 quantitatively, which was then deprotected to give 3′-C-(carbamoylmethyl)uridine (33).
- Ichikawa, Satoshi,Shuto, Satoshi,Minakawa, Noriaki,Matsuda, Akira
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p. 1368 - 1375
(2007/10/03)
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