Acetic Anhydride → 3,5-Dioxohexanoic acid

HRID 223522

반응식

HRID 223522 반응식
Cl.C([C:4]1[C:9]([OH:10])=[C:8]([CH2:11][OH:12])C(CO)=CN=1)=O.C(N(CC)CC)C.C([O:25][C:26](=[O:28])[CH3:27])(=O)C>O1CCCC1>[CH3:4][C:9]([CH2:8][C:11]([CH2:27][C:26]([OH:25])=[O:28])=[O:12])=[O:10]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 887065932-Formyl-3-hydroxy-4,5-dihydroxymethylpyridine hydrochloride

생성물 1

HCID 54598443,5-Dioxohexanoic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-379862411fe243c993bcfb596c0d74af
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04355034

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