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

HRID 52244

反応式

HRID 52244 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-ba6c218d0dfa458986e4da9c49c716cb
出典データセット
uspto-grants-1997_04
特許番号
US05616594

関連ノート

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