Acetic Anhydride → 2-(4-fluorophenyl)-5-methyl-2H-1,2,3-triazol-4-yl acetate

HRID 623694노트

반응식

HRID 623694 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[N:12]=[C:11]([CH3:13])[CH:10]=[N+:9]2[O-])=[CH:4][CH:3]=1.[C:15]([O:18]C(=O)C)(=[O:17])[CH3:16]>>[C:15]([O:18][C:10]1[C:11]([CH3:13])=[N:12][N:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[N:9]=1)(=[O:17])[CH3:16]

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 901115092-(4-fluorophenyl)-4-methyl-2H-1,2,3-triazole 1-oxide2회

생성물 1

HCID 901095002-(4-fluorophenyl)-5-methyl-2H-1,2,3-triazol-4-yl acetate

실험 절차

2-(4-Fluorophenyl)-4-methyl-2H-1,2,3-triazole 1-oxide (i.e. the product of Step A, 6.6 g, 34 mmol) was added to acetic anhydride (47 mL, 500 mmol), and the reaction mixture was stirred at reflux for 28 h. The reaction was concentrated under reduced pressure. The residue was taken up in ethyl acetate, washed successively with water and saturated aqueous sodium chloride solution, dried with magnesium sulfate and concentrated under reduced pressure to afford the title compound (7.8 g) as a beige solid. The title compound was used directly in the next step without further purification.

후처리

  1. temperatureat reflux for 28 h
  2. concentrationThe reaction was concentrated under reduced pressure
  3. washwashed successively with water and saturated aqueous sodium chloride solution
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-b48e8abb97ed4654b32961d88556da64
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302999B2

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