- Preparation method of 3-oxetanecarboxylic acid
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The invention provides a preparation method of 3-oxetanecarboxylic acid. According to the preparation method, 2-hydroxymethyl-2-nitro-1,3-propylene glycol is taken as a raw material, hydroxyl in 2-hydroxymethyl-2-nitro-1,3-propylene glycol is subjected to a group protection reaction, nitryl in 2-hydroxymethyl-2-nitro-1,3-propylene glycol is subjected to a reductive elimination reaction and hydrolysis reaction, and 2-hydroxymethyl-1,3-propylene glycol is obtained; 2-hydroxymethyl-1,3-propylene glycol is continuously subjected to a cyclization reaction and an oxidation reaction, and 3-oxetanecarboxylic acid is obtained. The provided preparation method can be completed only through five-step reactions; compared with existing preparation methods through ten-step reactions, the preparation method has the advantages that the reaction steps are greatly reduced, the reaction routes are greatly shortened, the overall yield is increased, and the final yield can be up to 50% or above on the basisof the raw material, namely, 2-hydroxymethyl-2-nitro-1,3-propylene glycol; the related reactions are simple, and the method is easy to operate and favorable for industrial production.
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Paragraph 0066; 0068-0070; 0092; 0114
(2018/09/12)
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- Simple Syntheses of 2-Hydroxymethyl-1,3-propanediol and Related Compounds
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A significantly improved synthesis of 2-hydroxymethyl-1,3-propanediol involves benzoylation of 2-hydroxymethyl-2-nitro-1,3-propanediol, replacement of the nitro group by hydrogen using tributylstannane, and methanolysis.Other simple procedures yield the corresponding trimethanesulfonate, triiodide, and trichloride.Dehydrohalogenation of the triiodide and the trichloride by DBU provides 3-iodo-2-(iodomethyl)propene and the corresponding dichloride, respectively.All of these useful compounds are now readily available for the first time.
- Latour, Stephan,Wuest, James D.
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p. 742 - 744
(2007/10/02)
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