Potassium Iodide → 1-{3-[4-[Bis(4-fluorophenyl)methylene]piperidino]propyl}-4-(2-pyrimidinyl)piperazine dihydrochloride

HRID 1460449ノート

反応式

HRID 1460449 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH2:7][CH2:6]1.[F:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]([C:31]2[CH:36]=[CH:35][C:34]([F:37])=[CH:33][CH:32]=2)=[C:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)CC(=O)C>[ClH:1].[ClH:1].[F:37][C:34]1[CH:35]=[CH:36][C:31]([C:24]([C:21]2[CH:20]=[CH:19][C:18]([F:17])=[CH:23][CH:22]=2)=[C:25]2[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][CH2:4][N:5]3[CH2:10][CH2:9][N:8]([C:11]4[N:16]=[CH:15][CH:14]=[CH:13][N:12]=4)[CH2:7][CH2:6]3)[CH2:27][CH2:26]2)=[CH:32][CH:33]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 27244364-(Bis(4-fluorophenyl)methylene)piperidineHCID 148827373-[4-(2-Pyrimidinyl)piperazinyl]propyl chloride

生成物 1

HCID 199157831-{3-[4-[Bis(4-fluorophenyl)methylene]piperidino]propyl}-4-(2-pyrimidinyl)piperazine dihydrochloride

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A mixture of 0.89 g of 1-(3-chloropropyl)-4-(2-pyrimidinyl)piperazine, 0.80 g of 4-[bis(4-fluorophenyl)methylene]piperidine and 0.51 g of potassium carbonate in 30 ml of 4-methyl-2-pentanone is brought to reflux for 48 hours in the presence of a trace of potassium iodide. The solvent is evaporated off and the residue is taken up in dichloromethane. The solution is washed with water. It is concentrated. The residue obtained is purified on a silica column using a mixture of dichloromethane and methanol (80:20 V/V) as eluent.

後処理

  1. customThe solvent is evaporated off
  2. washThe solution is washed with water
  3. concentrationIt is concentrated
  4. customThe residue obtained
  5. customis purified on a silica column
  6. additiona mixture of dichloromethane and methanol (80:20 V/V) as eluent

出典と根拠

ORDレコード
ord-cdf4ecfb43b6478e81a937b37aff5d71
出典データセット
uspto-grants-1991_12
特許番号
US05071847

反応ノート

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