Ethyl Acetate → 3-(2-chloro-6-fluorophenyl)-5-(3-chloro 4-hydroxymethylphenyl)-1-methyl-1H-1,2,4-triazole

HRID 1940744

반응식

HRID 1940744 반응식
C([O:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:16]([CH3:17])[N:15]=[C:14]([C:18]3[C:23]([F:24])=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:25])[N:13]=2)=[CH:8][C:7]=1[Cl:26])(=O)C.[OH-].[Na+].C(OCC)(=O)C>C(O)C.O>[Cl:25][C:19]1[CH:20]=[CH:21][CH:22]=[C:23]([F:24])[C:18]=1[C:14]1[N:13]=[C:12]([C:9]2[CH:10]=[CH:11][C:6]([CH2:5][OH:4])=[C:7]([Cl:26])[CH:8]=2)[N:16]([CH3:17])[N:15]=1

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 214636815-(4-acetoxymethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl) 1-methyl-1H-1,2,4-triazole

생성물 1

HCID 214636723-(2-chloro-6-fluorophenyl)-5-(3-chloro 4-hydroxymethylphenyl)-1-methyl-1H-1,2,4-triazole수율 67.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

5-(4-acetoxymethyl-3-chlorophenyl)-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole (11.1 g) is dissolved in a mixed solvent of ethanol (50 ml) and water (20 ml), added with sodium hydroxide (2.3 g) and heated under reflux for 1 hour with stirring. After cooling to room temperature, the reaction mixture is added with ethyl acetate and washed with water. Then, it is dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain crude solid. The crude solid is washed with mixed solvent of hexane-ethanol to give 6.7 g of desired compound (melting point: 111°-113° C.).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. washwashed with water
  4. dry with materialThen, it is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto obtain crude solid
  7. washThe crude solid is washed with mixed solvent of hexane-ethanol

출처 및 근거

ORD 기록
ord-ec1c00978d414858b10746b080e24413
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700824

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