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Ethanol → 1-(2-Fluoro-4-chloro-5-methylsulfonyloxyphenyl)-3,4,5-trimethylpyrazole

HRID 580254
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HRID 580254 반응식
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][S:10]([CH3:13])(=[O:12])=[O:11])=[CH:4][C:3]=1[NH:14][NH2:15].[CH3:16][C:17]([CH:19]([C:21]([CH3:23])=O)[CH3:20])=O.C(O)C.O>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][S:10]([CH3:13])(=[O:11])=[O:12])=[CH:4][C:3]=1[N:14]1[C:21]([CH3:23])=[C:19]([CH3:20])[C:17]([CH3:16])=[N:15]1
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참가 물질

6

반응물 4

HCID 702EthanolHCID 962WaterHCID 699493-Methyl-2,4-pentanedioneHCID 137982312-Fluoro-4-chloro-5-methylsulfonyloxyphenylhydrazine

생성물 1

HCID 137982321-(2-Fluoro-4-chloro-5-methylsulfonyloxyphenyl)-3,4,5-trimethylpyrazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of (2-fluoro-4-chloro-5-methylsulfonyloxyphenyl)hydrazine (25.5 g) of the formula: ##STR53## 3-methylpenta-2,5-dione (CH3COCH(CH3)COCH3) (11.4 g), ethanol (100 ml) and water (100 ml) was heated to reflux for one hour. After the reaction mixture was cooled, toluene was added thereto to form two layers. The toluene layer separated was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent by distillation in vacuo gave the titled compound (29.3 g) as a pale yellow crystalline solid. Recrystallization of this solid from a mixture of n-hexane and ethyl acetate afforded a white crystalline solid. m.p. 123°-125° C.

후처리

  1. temperatureto reflux for one hour
  2. temperatureAfter the reaction mixture was cooled
  3. customto form two layers
  4. customThe toluene layer separated
  5. washwas washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customRemoval of the solvent
  8. distillationby distillation in vacuo

출처 및 근거

ORD 기록
ord-d934f44226454b649bf88336f863f365
출처 데이터셋
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04752326

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