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Acetic Anhydride → 3,5-Dioxohexanoic acid

HRID 223522
ノート
印刷プレビュー

反応式

HRID 223522 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 54598443,5-Dioxohexanoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

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

反応ノート

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