Dimethylformamide → 5-(4-acetoxymethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole

HRID 52243

반응식

HRID 52243 반응식
CN(C)C=O.Br[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:18]([CH3:19])[N:17]=[C:16]([C:20]3[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=3[Cl:27])[N:15]=2)=[CH:10][C:9]=1[Cl:28].[C:29]([O-:32])(=[O:31])[CH3:30].[K+]>O>[C:29]([O:32][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:18]([CH3:19])[N:17]=[C:16]([C:20]3[C:25]([F:26])=[CH:24][CH:23]=[CH:22][C:21]=3[Cl:27])[N:15]=2)=[CH:10][C:9]=1[Cl:28])(=[O:31])[CH3:30]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 517044Potassium AcetateHCID 214636485-(4-bromomethyl-3-chlorophenyl) 3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole

생성물 1

HCID 214636815-(4-acetoxymethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole수율 51.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

To N,N-dimethylformamide (200 ml) are added 5-(4-bromomethyl-3-chlorophenyl)-3(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (24.3 g) and potassium acetate (29.0 g), which are stirred at 130° C. for 3 hours. The reaction mixture is cooled to room temperature, poured into water and extracted with ethyl acetate. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexaneethyl acetate as eluent to give 11.8 g of desired compound.

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer is washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe concentrate is purified by silica gel column chromatography
  7. additionusing mixed solvent of hexaneethyl acetate as eluent

출처 및 근거

ORD 기록
ord-8fa665d60d0042bb9c1b74ac3290d927
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616594

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