Pyrazole → 1-(2,6-Dichloro-4-nitrophenyl)-pyrazole

HRID 1709694

反応式

HRID 1709694 の反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[H-].[Na+].[Cl:8][C:9]1[CH:10]=[C:11]([N+:17]([O-:19])=[O:18])[CH:12]=[C:13]([Cl:16])[C:14]=1F>CN(C=O)C>[Cl:8][C:9]1[CH:10]=[C:11]([N+:17]([O-:19])=[O:18])[CH:12]=[C:13]([Cl:16])[C:14]=1[N:1]1[CH:5]=[CH:4][CH:3]=[N:2]1

参加物

5

反応物 3

HCID 1048PyrazoleHCID 24758Sodium hydrideHCID 765541,3-Dichloro-2-fluoro-5-nitrobenzene

生成物 1

HCID 230365521-(2,6-Dichloro-4-nitrophenyl)-pyrazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

実験手順

Pyrazole (1.43 g, 21,0 mmol) in 3 ml of DMF is added dropwise at RT to a suspension of sodium hydride (50%; 1.0 g, 21.0 mmol) in 10 ml of DMF. The mixture is stirred at RT for 30 min., after which it is added dropwise at 5° over a period of 30 min. to a solution of 3,5-dichloro-4-fluoronitrobenzene (3.0 g, 15.0 mmol) in 20 ml of DMF. After reaction is complete, the reaction mixture is quenched with water and extracted with ethyl acetate. The combined organic layers are washed with water and with brine and dried to give a yellow solid, 1-(2,6-dichloro-4-nitrophenyl)-pyrazole.

後処理

  1. customAfter reaction
  2. customthe reaction mixture is quenched with water
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layers are washed with water and with brine
  5. customdried

出典と根拠

ORDレコード
ord-e9cf5a8757d7446da8ef330c5a36ec4c
出典データセット
uspto-grants-1990_08
特許番号
US04950678

関連ノート

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