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

HRID 580254
ノート
印刷プレビュー

反応式

HRID 580254 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d934f44226454b649bf88336f863f365
出典データセット
uspto-grants-1988_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04752326

反応ノート

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