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Acetic Anhydride → HCID 18182171、化合物

HRID 1359259
ノート
印刷プレビュー

反応式

HRID 1359259 の反応式
[OH:1][CH:2]([C:9]1[CH:14]=[CH:13][N:12]=[C:11]([O:15][CH3:16])[CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:17](OC(=O)C)(=[O:19])[CH3:18]>N1C=CC=CC=1>[C:17]([O:1][CH:2]([C:9]1[CH:14]=[CH:13][N:12]=[C:11]([O:15][CH3:16])[CH:10]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1)(=[O:19])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 181824412-Methoxy-α-phenyl-4-pyridinemethanol

生成物 1

HCID 18182171HCID 18182171、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 104 g of 4-(α-hydroxybenzyl)-2-methoxypyridine, 100 ml of acetic acid anhydride and 100 ml of pyridine was heated under stirring for 5 hours in an oil bath kept at 110° C. After the reaction solution was evaporated, water was added to the residue and the mixture was extracted with ethyl acetate. The extract was washed with an aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography using 5-20% ethyl acetate/hexane, to give 112 g of the target compound.

後処理

  1. temperaturewas heated
  2. customkept at 110° C
  3. customAfter the reaction solution was evaporated
  4. additionwater was added to the residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with an aqueous sodium bicarbonate solution and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was removed

出典と根拠

ORDレコード
ord-ca3880a2a0fd48c1b21950925e7f6896
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599917B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート