Water → 1-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

HRID 13187

반응식

HRID 13187 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=O.C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=[N:9][NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 69982(4-Fluorophenyl)hydrazineHCID 27348722-Fluoro-5-methoxybenzaldehyde

생성물 1

HCID 668125981-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

(4-fluorophenyl)hydrazine (6.5 g, 40 mmol), 2-fluoro-5-methoxybenzaldehyde (6.2 g, 40 mmol) and cesium carbonate (13 g, 40 mmol) were stirred in DMF (40 mL) at r.t. under argon atmosphere for 1.5 h and was then poured with stirring into water and extracted with ethyl acetate. The organic phase was washed trice with water, then brine and evaporated. The residue crystallized slowly to afford the subtitle compound as a beige-light brown crystal mass (10.21 g).

후처리

  1. additionwas then poured
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed trice with water
  4. custombrine and evaporated
  5. customThe residue crystallized slowly

출처 및 근거

ORD 기록
ord-5de05775b2444b41b706539db408683e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728030B2

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