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

HRID 1460449노트

반응식

HRID 1460449 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cdf4ecfb43b6478e81a937b37aff5d71
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05071847

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