Electric Literature of 15568-85-1, A common heterocyclic compound, 15568-85-1, name is 5-(Methoxymethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione, molecular formula is C8H10O5, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step 3[00178] To a stirred solution of the l-(3,4-dichloro-phenyl)-ethanone oxime (1 eq) in dry THF (6vol) cooled externally to -15C was added 2.5M n-BuLi (2.2 eq) dropwise. After stirring the reaction mixture for 75 minutes, 5-methoxymethylene- 2,2-dimethyl-[l,3]dioxane-4,6-dione (1.0 eq) in THF (9 vol) was added to the externally cooled reaction mixture. After 1 hour the reaction mixture was warmed to 0C for 15 minutes, and then stirred for 16 hours at room temperature. The reaction mixture was added to water (27vol) and extracted with TBME (2 x 7vol). The aqueous layer was acidified with 5M H2SO4 (3vol) and further extracted with TMBE (3 x 7 vol). The combined organics were filtered and concentrated under reduced pressure to give a crude residue.
The synthetic route of 15568-85-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; CHDI, INC.; WITYAK, John; TOLEDO-SHERMAN, Leticia, M.; LEEDS, Janet; DOMINGUEZ, Celia; COURTNEY, Stephen, Martin; YARNOLD, Christopher, John; DE AGUIAR PENA, Paula, Cristina; SCHEEL, Andreas; WINKLER, Dirk; WO2010/17132; (2010); A1;,
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