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

HRID 1940744

反応式

HRID 1940744 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-ec1c00978d414858b10746b080e24413
出典データセット
uspto-grants-1997_12
特許番号
US05700824

関連ノート

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