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Potassium Carbonate → HCID 21070994、化合物

HRID 1372133
ノート
印刷プレビュー

反応式

HRID 1372133 の反応式
[CH3:1][C:2]1[NH:3][CH:4]=[C:5]([CH3:7])[N:6]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=2)[CH2:20][CH2:19]1)=[O:17]>CN(C=O)C>[Cl:30][C:27]1[CH:26]=[CH:25][C:24]([N:21]2[CH2:20][CH2:19][N:18]([C:16](=[O:17])[CH2:15][N:3]3[CH:4]=[C:5]([CH3:7])[N:6]=[C:2]3[CH3:1])[CH2:23][CH2:22]2)=[CH:29][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 40539571-(Chloroacetyl)-4-(4-chlorophenyl)piperazineHCID 178430880HCID 178430880、化合物

生成物 1

HCID 21070994HCID 21070994、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

2,4-dimethylimidazole (0.633 g, 0.7 mmol) was taken up in dry DMF (15 ml) and dry potassium carbonate (340 mg) and KI (20 mg) was added and the reaction mixture was stirred at room temperature for 1 h under nitrogen. 2-Chloro-1-[4-(4-chloro-phenyl)-piperazin-1-yl]-ethanone (200 mg, 1.1 mmol) in DMF (5 ml) was then added to the mixture through a syringe. The reaction was then heated at 140° C. for 14 h, cooled and quenched with water and extracted with ethyl acetate. Drying of the organic layer with Na2SO4 followed by concentration gave material that was purified on a silica gel column (CHCl3/MeOH): 1H NMR (300 MHz, CDCl3): δ 7.25 (d, 2H), 6.80 (d, 2H), 6.53 (s, 1H), 4.62 (s, 2H), 3.78 (br, 2H), 3.59 (br, 2H), 3.21 (br, 4H), 2.31 (s, 3H), 2.17 (s, 1H).

後処理

  1. temperatureThe reaction was then heated at 140° C. for 14 h
  2. temperaturecooled
  3. customquenched with water
  4. extractionextracted with ethyl acetate
  5. dry with materialDrying of the organic layer with Na2SO4
  6. concentrationfollowed by concentration
  7. customgave material that
  8. customwas purified on a silica gel column (CHCl3/MeOH)

出典と根拠

ORDレコード
ord-1d378128d4b549c296ebf446ece96e28
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157464B2

反応ノート

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