Water → HCID 18357129、化合物

HRID 427449

反応式

HRID 427449 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)=[CH:3][CH:2]=1.F[C:14]1[CH:27]=[CH:26][C:17]([C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:19])=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[C:18]([C:20]1[CH:25]=[CH:24][C:23]([N:10]2[CH2:9][CH2:8][N:7]([C:4]3[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=3)[CH2:12][CH2:11]2)=[CH:22][CH:21]=1)(=[O:19])[C:17]1[CH:26]=[CH:27][CH:14]=[CH:15][CH:16]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 676634-FluorobenzophenoneHCID 705171-(4-Pyridyl)piperazine

生成物 1

HCID 18357129HCID 18357129、化合物収率 26.2%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A solution of N-(4-pyridyl)piperazine (815 mg), 4-fluorobenzophenone (1.2 g) and powdered potassium carbonate (912 mg) was stirred at 95° C. in DMSO (10 ml) overnight. The solution was poured into water (150 ml) and extracted with dichloromethane (3×50 ml). The dichloromethane extracts were combined, washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography on alumina (ICN Alumina N 32-63) using 1% methanol in dichloromethane as eluant to give a solid. The solid was recrystallised from a mixture of ethyl acetate/isohexane to give 1-(4-benzoylphenyl)-4-(4-pyridyl)piperazine (450 mg) as a solid. m.p.136-137° C.

後処理

  1. extractionextracted with dichloromethane (3×50 ml)
  2. washwashed with water
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by chromatography on alumina (ICN Alumina N 32-63)
  6. customto give a solid
  7. customThe solid was recrystallised from a mixture of ethyl acetate/isohexane

出典と根拠

ORDレコード
ord-f727f45183664540b591d773fc72606e
出典データセット
uspto-grants-2001_11
特許番号
US06313127B1

関連ノート

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