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

HRID 1446570
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HRID 1446570 반응식
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]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 836431-(2,6-Difluorophenyl)ethan-1-oneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 167683711-(2,6-Difluorophenyl)ethanamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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 %)

출처 및 근거

ORD 기록
ord-c963ce43129b445d8216f35f62a7db2b
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07667041B2

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