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Triethylamine → 1-(2,6-Difluorophenyl)ethanamine

HRID 1362714
ノート
印刷プレビュー

反応式

HRID 1362714 の反応式
C([N:3]([CH2:6][CH3:7])CC)C.Cl.NO.CC([C:14]1[C:19]([F:20])=[CH:18][CH:17]=[CH:16][C:15]=1[F:21])=O>C(O)C>[F:20][C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([F:21])[C:14]=1[CH:6]([NH2:3])[CH3:7]
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 8471TriethylamineHCID 836431-(2,6-Difluorophenyl)ethan-1-oneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 167683711-(2,6-Difluorophenyl)ethanamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Triethylamine (2.37 mL) and hydroxylamine hydrochloride (634 mg) were added to a solution of 2,6-difluoroacetophenone (890 mg) in ethanol (30 mL), and the reaction solution was heated to reflux for 4 hours. The reaction solution was returned to room temperature, and the solvent was evaporated under reduced pressure. Zinc (1.86 g) was added to a solution of the resulting residue in trifluoroacetic acid (10 mL), and the reaction solution was stirred at room temperature overnight. The reaction solution was filtered on a celite, made basic with a 5 N aqueous solution of sodium hydroxide, and then extracted with chloroform. The resulting organic layer was dried over magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 210 mg of a crude purified product containing the title compound (purity: 50 wt %). The physical properties of the compound are as follows.

後処理

  1. temperaturethe reaction solution was heated
  2. temperatureto reflux for 4 hours
  3. customwas returned to room temperature
  4. customthe solvent was evaporated under reduced pressure
  5. additionZinc (1.86 g) was added to a solution of the resulting residue in trifluoroacetic acid (10 mL)
  6. filtrationThe reaction solution was filtered on a celite
  7. extractionextracted with chloroform
  8. dry with materialThe resulting organic layer was dried over magnesium sulfate
  9. customthe solvent was evaporated under reduced pressure
  10. customto obtain 210 mg of a crude
  11. custompurified product
  12. additioncontaining the title compound (purity: 50 wt %)

出典と根拠

ORDレコード
ord-6b67e1a4f10e4e6e895e229c5a6f8360
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07880009B2

反応ノート

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