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

HRID 1440138노트

반응식

HRID 1440138 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 25134Boron tribromide3회HCID 186156481-Methyl-3-(2-fluoro-4-chloro-5-methoxyphenyl)-4-chloro-5-trifluoromethyl-1H-pyrazole

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-43d93fa907824359883bb3ec634c3c96
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496956

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