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Chlorine → ethyl 4-chloro-5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-3-carboxylate

HRID 254816
ノート
印刷プレビュー

反応式

HRID 254816 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:9]=2)=[CH:4][CH:3]=1.[Cl:26]Cl>C(O)(=O)C>[Cl:26][C:9]1[C:10]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[N:11][N:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[C:8]=1[C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24526ChlorineHCID 10905332Ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1h-pyrazole-3-carboxylate

生成物 1

HCID 66844323ethyl 4-chloro-5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-3-carboxylate収率 95%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of ethyl 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-1H-pyrazole-3-carboxylate (3.0 g, 7.6 mmol) in acetic acid (30 ml) at room temperature was bubbled chlorine gas for 10 minutes. The reaction mixture was stirred at room temperature for 2 hours and the resulting solution was quenched with water (100 ml). The organic solution was extracted with diethyl ether (100 ml×2). With saturated sodium bicarbonate solution, remained acetic acid was removed and organic phase was evaporated with reduced pressure. The crude residue was purified with silica gel column (hexane/ethyl acetate=5/1) to produce title compound (3.1 g, 95% yield) as white solid.

後処理

  1. customthe resulting solution was quenched with water (100 ml)
  2. extractionThe organic solution was extracted with diethyl ether (100 ml×2)
  3. customwas removed
  4. customorganic phase was evaporated with reduced pressure
  5. customThe crude residue was purified with silica gel column (hexane/ethyl acetate=5/1)

出典と根拠

ORDレコード
ord-8d6a999b64d34c38989933b26f8941ea
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07875647B2

反応ノート

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