Water → 6-(4-Bromophenyl)-3-(2,6-difluorophenyl)-[1,2,4]triazine

HRID 2085918노트

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HRID 2085918 반응식
C(OC([NH:8][NH:9][C:10]([C:12]1[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=1[F:19])=N)=O)(C)(C)C.[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:27](=O)[CH:28]=[N:29]O)=[CH:23][CH:22]=1.C([O-])(=O)C.[Na+].O>C(O)(=O)C>[Br:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[N:8]=[N:9][C:10]([C:12]3[C:13]([F:19])=[CH:14][CH:15]=[CH:16][C:17]=3[F:18])=[N:29][CH:28]=2)=[CH:23][CH:22]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 517045Sodium AcetateHCID 72814957(4-Bromo-phenyl)-oxo-acetaldehyde oximeHCID 178454364HCID 178454364, 화합물

생성물 1

HCID 227270186-(4-Bromophenyl)-3-(2,6-difluorophenyl)-[1,2,4]triazine

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
10 °C

실험 절차

A mixture of 200 mg of N′-[(2,6-difluorophenyl)-iminomethyl]-hydrazinecarboxylic acid tert-butyl ester, 114 mg of (4-bromophenyl)-oxoacetaldehyde oxime and 123 mg of sodium acetate in 1.5 ml of glacial acetic acid is heated at 10° C. for 3 h. After cooling to room temperature, the reaction mixture is poured into water and extracted with ethyl acetate. The organic phase is washed in succession with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The residue is purified by means of flash chromatography (1% methanol in dichloromethane). In this way the title compound having a melting point of 180-181° C. is obtained.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic phase is washed in succession with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue is purified by means of flash chromatography (1% methanol in dichloromethane)
  8. customis obtained

출처 및 근거

ORD 기록
ord-752c34a7b7354a6fa46ce6e7d9bcd369
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723720B2

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