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Acetic Anhydride → 5,6,7,8-Tetrahydroquinolin-8-yl acetate

HRID 2301140
ノート
印刷プレビュー

反応式

HRID 2301140 の反応式
[N+:1]1([O-])[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:12]([O:15]C(=O)C)(=[O:14])[CH3:13]>>[C:12]([O:15][CH:9]1[C:10]2[N:1]=[CH:2][CH:3]=[CH:4][C:5]=2[CH2:6][CH2:7][CH2:8]1)(=[O:14])[CH3:13]
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

3

反応物 2

HCID 7918Acetic AnhydrideHCID 27781345,6,7,8-Tetrahydro-1-quinoliniumolate

生成物 1

HCID 122262495,6,7,8-Tetrahydroquinolin-8-yl acetate収率 33%

反応条件

温度
90 °C

実験手順

5,6,7,8-Tetrahydroquinoline N-oxide (1.6 g, 11 mmol) was mixed with acetic anhydride (9.2 ml) and stirred at 90° C. for 7 hours. After removing the solvent by evaporation under a reduced pressure, the residue was neutralized with sodium hydroxide aqueous solution (1 N) and the reaction product was extracted with chloroform. The extract was washed with saturated brine and dried with anhydrous sodium sulfate, and then the solvent was removed by evaporation under a reduced pressure and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 690 mg (3.6 mmol, 33%) of the title compound.

後処理

  1. customAfter removing the solvent
  2. customby evaporation under a reduced pressure
  3. extractionthe reaction product was extracted with chloroform
  4. washThe extract was washed with saturated brine
  5. dry with materialdried with anhydrous sodium sulfate
  6. customthe solvent was removed by evaporation under a reduced pressure
  7. customthe thus obtained material was separated
  8. custompurified by a silica gel column chromatography

出典と根拠

ORDレコード
ord-63fbf13115b54df1b80ed99559a6b0e5
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498251B1

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