1-(2-Methoxyphenyl)piperazine → HCID 24205899、化合物

HRID 1944988ノート

反応式

HRID 1944988 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:12])[CH2:10]Cl)=[C:4]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:28][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[N:36]1[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]1>CC(C)=O.C(OCC)(=O)C.CCCCCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:12])[CH2:10][N:39]2[CH2:38][CH2:37][N:36]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=3[O:29][CH3:28])[CH2:41][CH2:40]2)=[C:4]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[CH:3]=1

参加物

6

反応物 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 11430Potassium CarbonateHCID 844102,4'-Dichloro-2'-o-chlorobenzoylacetanilide

生成物 1

HCID 24205899HCID 24205899、化合物収率 89.9%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 21226206Ethyl acetate hexane溶媒

実験手順

To a compound of N1-[4-chloro-2-(2-chlorobenzoyl)phenyl]-2-chloroacetamide (600 mg, 1.74 mmol) in dry acetone (20 mL) was added anhydrous potassium carbonate (1.21 g, 8.78 mmol) and 1-(2-methoxyphenyl)piperazine (336 mg, 1.98 mmol). The reaction mixture was refluxed for 24 h and the reaction was monitored by TLC using ethyl acetate-hexane (6:4) as a solvent system. The potassium carbonate was then removed by suction filtration and the solvent was evaporated under vacuum to afford the crude product. This was further purified by column chromatography using ethyl acetate:hexane (6:4) as a solvent system to obtain the pure product 6c (780 mg, 89% yield).

後処理

  1. temperatureThe reaction mixture was refluxed for 24 h
  2. customThe potassium carbonate was then removed by suction filtration
  3. customthe solvent was evaporated under vacuum
  4. customto afford the crude product
  5. customThis was further purified by column chromatography

出典と根拠

ORDレコード
ord-08d10e2641a94022bd952ca1ea5861fb
出典データセット
uspto-grants-2013_03
特許番号
US08394954B2

反応ノート

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