Acetic Anhydride → 3,5-Dioxohexanoic acid

A solution of one equivalent of 2-formyl-3-hydroxy-4,5-dihydroxymethylpyridine hydrochloride in 400 ml. anhydrous tetrahydrofuran is treated with four equivalents of triethylamine and aged for one hour at room temperature. Then three equivalents of acetic anhydride are introduced, and the reaction mixture is aged 4 hours at room temperature. The reaction mixture is concentrated under reduced pressure to a gum. This is treated with a mixture of 300 ml. of diethyl ether and 300 ml. of distilled water. After shaking well, the layers are separated and the ether layer is dried over magnesium sulfate. After evaporation to dryness, the desired triacetate is obtained as a viscous oil.

1. waitthe reaction mixture is aged 4 hours at room temperature
2. concentrationThe reaction mixture is concentrated under reduced pressure to a gum
3. additionThis is treated with a mixture of 300 ml
4. customthe layers are separated
5. dry with materialthe ether layer is dried over magnesium sulfate
6. customAfter evaporation to dryness

ORDレコード

ord-379862411fe243c993bcfb596c0d74af

出典データセット

uspto-grants-1982_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04355034