95579-71-8Relevant articles and documents
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.
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