Hydrazine → 2,4-Dimethoxybenzohydrazide

HRID 10731

반응식

HRID 10731 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:5]=1[O:12][CH3:13].[NH2:15][NH2:16]>CO>[CH3:13][O:12][C:5]1[CH:6]=[C:7]([O:10][CH3:11])[CH:8]=[CH:9][C:4]=1[C:3]([NH:15][NH2:16])=[O:2]

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 137451Benzoic acid, 2,4-dimethoxy-, methyl ester

생성물 1

HCID 4567282,4-Dimethoxybenzohydrazide수율 78.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Ex-109A: A solution of 2,4-dimethoxy-benzoic acid methyl ester (4.24 g, 21.6 mmol) and hydrazine (3.4 mL, 108.1 mmol) in methanol (50 mL) was refluxed overnight. Solvent was removed under reduced pressure. The residue was re-dissolved in ethyl acetate. The solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine, dried over sodium carbonate and concentrated to afford 2,4-dimethoxy-benzoic acid hydrazide (3.31 g, 78%) as a white solid: 1H NMR (CDCl3) δ 8.77 (bs, 1H), 8.15 (d, J=8.8 Hz, 1H), 6.58 (dd, J=8.8, 2.2 Hz, 1H), 6.46 (d, J=2.2 Hz, 1H), 4.10 (bs, 2H), 3.91 (s, 3H), 3.83 (s, 3H).

후처리

  1. customSolvent was removed under reduced pressure
  2. dissolutionThe residue was re-dissolved in ethyl acetate
  3. washThe solution of ethyl acetate was washed with saturated solution of sodium bicarbonate and brine
  4. dry with materialdried over sodium carbonate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-665a71c8df494a06987f1f3e49f3c7d1
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094801B2

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