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Potassium Carbonate → HCID 21070994, 화합물

HRID 270917
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HRID 270917 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 40539571-(Chloroacetyl)-4-(4-chlorophenyl)piperazineHCID 178430880HCID 178430880, 화합물

생성물 1

HCID 21070994HCID 21070994, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-4393d85e1b194925a3bbd949b0817fd6
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07449576B1

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