Water → 4-Chloro-3-(4-chloro-2-fluoro-5-hydroxyphenyl)-1-methyl-5-trifluoromethyl-1H-pyrazole

HRID 260956ノート

反応式

HRID 260956 の反応式
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[C:16]([O:18]C)[C:15]([Cl:20])=[CH:14][C:13]=2[F:21])=[N:4][N:5]([CH3:11])[C:6]=1[C:7]([F:10])([F:9])[F:8].B(Br)(Br)Br.O>C(Cl)Cl>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[C:16]([OH:18])[C:15]([Cl:20])=[CH:14][C:13]=2[F:21])=[N:4][N:5]([CH3:11])[C:6]=1[C:7]([F:9])([F:8])[F:10]

参加物

5

反応物 3

HCID 962WaterHCID 25134Boron tribromide3 回HCID 186156481-Methyl-3-(2-fluoro-4-chloro-5-methoxyphenyl)-4-chloro-5-trifluoromethyl-1H-pyrazole

生成物 1

HCID 111210244-Chloro-3-(4-chloro-2-fluoro-5-hydroxyphenyl)-1-methyl-5-trifluoromethyl-1H-pyrazole収率 96%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.39 g of 4-chloro-3-(4-chloro-2-fluoro-5-methoxyphenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole was dissolved in 80 ml of anhydrous methylene chloride and then cooled with a dry ice/acetone bath and 0.14 ml of boron tribromide added. After allowing to warm to room temperature, the mixture was treated with an additional 0.28 ml of boron tribromide. Added was an additional 1.0 ml of boron tribromide and stirred at room temperature for 6 hours. After stirring, 30-50 ml of ice cooled water was added and the mixture stirred for 10 minutes. The organic phase was extracted with water, dried with anhydrous magnesium sulfate, filtered and concentrated to give 1.28 g of 4-chloro-3-(4-chloro-2-fluoro-5-hydroxyphenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole, m.p. 123.0°-126.0° C.

後処理

  1. temperaturecooled with a dry ice/acetone bath
  2. additionAdded
  3. stirringAfter stirring
  4. additionwas added
  5. stirringthe mixture stirred for 10 minutes
  6. extractionThe organic phase was extracted with water
  7. dry with materialdried with anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-efa216b6c140438cb643f22bbbe3c65d
出典データセット
uspto-grants-1996_06
特許番号
US05530126

反応ノート

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