95579-71-8Relevant academic research and scientific papers
A 4 - chloro methyl -5 - methyl - 1, 3 - dioxo heterocyclic pentene -2 - one purification method
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Paragraph 0023-0050, (2019/03/21)
The invention discloses a purification method of 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone. The purification method comprises the following steps of dissolving a crude product of 4-chloromethyl group-5-methyl-1,3-dioxole-2-ketone into a mixed solvent of methyl alcohol, ethyl alcohol, isopropyl alcohol and tertiary butanol for crystallizing for 0-24 hours at a temperature of -10-0 DEG C, and filtering to acquire the 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone. The purification method has the characteristics of low cost, good refining effect, high yield, low requirement on equipment and simplicity and convenience in operation and is suitable for industrial production.
Synthetic method of 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone
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Paragraph 0002; 0016; 0017, (2016/10/07)
The invention relates to a synthetic method of 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone. The method comprises the following steps that 1, DMDO is dissolved in organic solvent, and heating reflux is conducted, wherein the mass-to-volume ratio of the DMDO to the organic solvent ranges from 1:5 to 1:9; 2, by keeping a reflux state, sulfonyl chloride is evenly and dropwise added within 1-4 h, after the sulfonyl chloride is dropwise added, heat preservation is conducted continuously for 2 h to enable the reaction to be completely conducted, wherein the mole ratio of the DMDO to the sulfonyl chloride ranges from 1:0.7 to 1:3.5; 3, after the reaction is completed, rotary evaporateion is conducted to remove the organic solvent; 4, solid free radical scavenger is added, the temperature is raised to 90 DEG C, rearrangement is conducted, and a crude product of 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone is obtained, wherein the dosage of the solid free radical scavenger is 0.5%-2% of the mass of the DMDO; 5, under the vacuum degree of 2 mmHg, distillation is conducted at the temperature ranging from 91 DEG C to 93 DEG C, and high-purity 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone is obtained. According to the synthetic method of the 4-chloromethyl-5-methyl-1,3-dioxole-2-ketone, the conversion efficiency of the product and the yield of a target product can be improved, the production cost is reduced, and good economic benefit is achieved.
A Convenient and Practical Preparation of 4-Chloromethyl-5-methyl-1,3-dioxol-2-one
Ikeda, Shoji,Takebe, Yasushi,Hirayama, Ryoichi,Sakamoto, Fumio,Iuchi, Koji,Tsukamoto, Goro
, p. 394 - 397 (2007/10/02)
A new synthetic method for 4-chloromethyl-5-methyl-1,3-dioxol-2-one (1c), which is useful for preparing prodrugs, has been developed.Ene-chlorination of 4,5-dimethyl-1,3-dioxol-2-one (2) with chlorine or sulfuryl chloride afforded 4-chloro-4-methyl-5-methylene-1,3-dioxolan-2-one (3) in good yield.Compound 3 underwent allylic rearrangement to afford 1c quantitatively.The overall yield of 1c from 2 was approximately 80percent. Keywords---4-chloromethyl-5-methyl-1,3-dioxol-2-one; 4,5-dimethyl-1,3-dioxol-2-one; 4-chloro-4-methyl-5-methylene-1,3-dioxolan-2-one; ene-chlorination; allylic rearrangement; (5-methyl-2-oxo-1,3-dioxol-4-yl)methyl group; promoiety; prodrug
4-Chloro-4-methyl-5-methylene-1,3-dioxolane-2-one
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, (2008/06/13)
4-Chloro-4-methyl-5-methylene-1,3-dioxolane-2-one is useful as an intermediate for the synthesis of 4-chloromethyl-5-methyl-1,3-dioxolene-2-one which, in turn, finds use as a modifying agent for making various prodrugs. Said intermediate compound gives said objective compound in a good yield by a rearrangement reaction.
