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Sodium Bicarbonate → 1-(3-Chloro-4-bromophenyl)-3-trifluoromethyl-4-fluoro-4-allyl-5-pyrazolone

HRID 1382661
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HRID 1382661 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12]([CH2:16][CH:17]=[CH2:18])(O)[C:11]([C:19]([F:22])([F:21])[F:20])=[N:10]2)[CH:5]=[CH:6][C:7]=1[Br:8].C(N(SN(CC)CC)CC)C.[F-:34].[F-].[F-].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12]([F:34])([CH2:16][CH:17]=[CH2:18])[C:11]([C:19]([F:22])([F:21])[F:20])=[N:10]2)[CH:5]=[CH:6][C:7]=1[Br:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 212728871-(3-Chloro-4-bromophenyl)-3-trifluoromethyl-4-allyl-4-hydroxy-5-pyrazoloneHCID 86605672Diethylaminosulfide trifluoride

생성물 1

HCID 212728901-(3-Chloro-4-bromophenyl)-3-trifluoromethyl-4-fluoro-4-allyl-5-pyrazolone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-3 °C

실험 절차

4 g of 1-(3-chloro-4-bromophenyl)-3-trifluoromethyl-4-allyl-4-hydroxy-5-pyrazolone in 200 ml of methylene chloride were cooled to -10° C. and 2.7 ml of trifluoride diethylaminosulfide were added all at once. The mixture was stirred for one hour at -10° C./-3° C. 120 ml of a saturated solution of sodium bicarbonate were added and stirring was carried out for 10 minutes, followed by decanting, washing with water, drying and bringing to dryness. The residue was chromatographed on silica and eluted with a hexane-methylene chloride mixture (8-2) to obtain 1.1 g of 1-(3-chloro-4-bromophenyl)-3-trifluoromethyl-4-fluoro-4-allyl-5-pyrazolone.

후처리

  1. stirringstirring
  2. waitwas carried out for 10 minutes
  3. customby decanting
  4. washwashing with water
  5. customdrying
  6. customThe residue was chromatographed on silica
  7. washeluted with a hexane-methylene chloride mixture (8-2)

출처 및 근거

ORD 기록
ord-212ae14063614531ad92884360c6a48f
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04808210

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