Triethylamine → 2,3-difluoro-N'-hydroxybenzenecarboximidamide

HRID 1642821노트

반응식

HRID 1642821 반응식
[F:1][C:2]1[C:9]([F:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[Cl-].[OH:12][NH3+:13].C(N(CC)CC)C>C(O)C>[F:1][C:2]1[C:9]([F:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4](=[N:13][OH:12])[NH2:5]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21645Hydroxylamine HClHCID 889352,3-Difluorobenzonitrile

생성물 1

HCID 32783782,3-difluoro-N'-hydroxybenzenecarboximidamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

5.0 g (35.2 mmol) of 2,3-difluorobenzonitrile were initially charged in 43 ml of ethanol, and a solution of 3.7 g (52.8 mmol) of hydroxylammonium chloride and 5.9 ml (4.3 g, 42.3 mmol) of triethylamine was added at RT. The reaction mixture was stirred at RT for 16 h, concentrated under reduced pressure, taken up in ethyl acetate and washed with saturated aqueous sodium bicarbonate solution. The organic extracts were dried over sodium sulphate, filtered and concentrated under reduced pressure. Yield: 5.7 g (94% of theory)

후처리

  1. concentrationconcentrated under reduced pressure
  2. washwashed with saturated aqueous sodium bicarbonate solution
  3. dry with materialThe organic extracts were dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-433983e8521842ed81758141f19f9966
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08119663B2

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