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Ethanol → 2-Hydroxymethyl-4-(3-methoxypropoxy)pyridine

HRID 609854
ノート
印刷プレビュー

反応式

HRID 609854 の反応式
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][N+:10]([O-])=[C:9]([CH3:14])[CH:8]=1.C([OH:17])C>C(OC(=O)C)(=O)C>[OH:17][CH2:14][C:9]1[CH:8]=[C:7]([O:6][CH2:5][CH2:4][CH2:3][O:2][CH3:1])[CH:12]=[CH:11][N:10]=1
参加物反応条件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 702EthanolHCID 151662164-(3-Methoxypropoxy)-2-methylpyridine 1-oxide

生成物 1

HCID 151662262-Hydroxymethyl-4-(3-methoxypropoxy)pyridine

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

反応条件

温度
90 °C

実験手順

4.05 g (0.02 mol) of 4-methoxypropoxy-2-methylpyridine 1-oxide was dissolved in 50 ml of acetic anhydride to obtain a solution. This solution was stirred at 90° C. for 0.5 hour and cooled, followed by the addition of ethanol. The obtained mixture was concentrated under a reduced pressure, followed by the addition of 150 ml of 1N hydrochloric acid. The obtained mixture was stirred at 100° C. for one hour, cooled, neutralized with sodium hydrogencarbonate and extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. Thus, 3.64 g of the title compound was obtained as a crude product.

後処理

  1. customto obtain a solution
  2. temperaturecooled
  3. concentrationThe obtained mixture was concentrated under a reduced pressure
  4. additionfollowed by the addition of 150 ml of 1N hydrochloric acid
  5. stirringThe obtained mixture was stirred at 100° C. for one hour
  6. temperaturecooled
  7. extractionextracted with chloroform
  8. dry with materialThe extract was dried over magnesium sulfate
  9. filtrationfiltered
  10. distillationThe filtrate was distilled
  11. customto remove the solvent

出典と根拠

ORDレコード
ord-0bf6943192c54ae79fb2d0bbaca3cf31
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998445

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート