1-(2-Nitrophenyl)piperazine → HCID 27007991、化合物

HRID 1810963ノート

反応式

HRID 1810963 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH2:8][C:9]([OH:11])=O)[N:3]=1.C(C1NC=CN=1)(C1NC=CN=1)=O.[N+:24]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1)([O-:26])=[O:25]>CN(C=O)C.CCOC(C)=O>[CH3:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH2:8][C:9]([N:36]2[CH2:37][CH2:38][N:33]([C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=3[N+:24]([O-:26])=[O:25])[CH2:34][CH2:35]2)=[O:11])[N:3]=1

参加物

6

反応物 3

HCID 1009491-(2-Nitrophenyl)piperazineHCID 572875(3,5-Dimethyl-1H-pyrazol-1-yl)acetic acidHCID 5250894Bis-(1H-imidazol-2-YL)-methanone

生成物 1

HCID 27007991HCID 27007991、化合物収率 64%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To (3,5-dimethyl-pyrazol-1-yl)-acetic acid (0.140 g, 0.908 mmol) in DMF is added carbonyl diimidazole (0.140 g, 0.863 mmol) in one portion. The mixture is stirred for 1 h. To this is added 1-(2-nitro-phenyl)-piperazine (0.197 g, 0.950 mmol). The mixture is stirred for 14 h and then diluted with 100 mL EtOAc. The reaction is quenched with 20 mL of saturated NH4Cl, washed with 2×20 mL of H2O and 1×20 mL of brine. The organic phase is dried (MgSO4), filtered and concentrated to give 2-(3,5-dimethyl-pyrazol-1-yl)-1-[4-(2-nitro-phenyl)-piperazin-1-yl]-ethanone in 64% yield.

後処理

  1. stirringThe mixture is stirred for 14 h
  2. customThe reaction is quenched with 20 mL of saturated NH4Cl
  3. washwashed with 2×20 mL of H2O and 1×20 mL of brine
  4. dry with materialThe organic phase is dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-d5cbc1d651ec4ba2922786484632b56e
出典データセット
uspto-grants-2013_01
特許番号
US08362249B2

反応ノート

読み込み中…