Aluminum(III) Chloride → HCID 136048655、化合物

HRID 52245ノート

反応式

HRID 52245 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([O:20]C)=[C:16]([Cl:22])[CH:15]=2)[N:11]([CH3:23])[N:10]=1.[Cl-].[Al+3].[Cl-].[Cl-]>C1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[C:16]([Cl:22])[CH:15]=2)[N:11]([CH3:23])[N:10]=1

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 214636823-(2-chloro-6-fluorophenyl)-5-(3-chloro-4-methoxyphenyl)-1-methyl-1H-1,2,4-triazole

生成物 1

HCID 136048655HCID 136048655、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To benzene (300 ml) are added the crude product of 3-(2-chloro-6-fluorophenyl)-5-(3-chloro-4-methoxyphenyl)-1-methyl 1H-1,2,4-triazole (70.5 g) and anhydrous aluminum chloride (80.0 g), which are heated under reflux for 3 hours with stirring. After cooling to room temperature, the reaction mixture is poured into ice water and extracted with toluene. The organic layer is washed with water, extracted with aqueous solution of 20% NaOH, and the aqueous layer is acidified by adding a concentrated sulfuric acid little by little while cooling with ice and extracted with ethyl acetate. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 64.2 g of desired compound.

後処理

  1. temperatureare heated
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with toluene
  4. washThe organic layer is washed with water
  5. extractionextracted with aqueous solution of 20% NaOH
  6. additionby adding a concentrated sulfuric acid little by little
  7. temperaturewhile cooling with ice
  8. extractionextracted with ethyl acetate
  9. washThe organic layer is washed with water
  10. dry with materialdried over anhydrous magnesium sulfate
  11. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a7c3eb304c44496ba5ff4c3a302ccbf0
出典データセット
uspto-grants-1997_04
特許番号
US05616594

反応ノート

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