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Potassium Carbonate → HCID 68538008, 화합물

HRID 1993706
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HRID 1993706 반응식
[C:1]([C:5]1[CH:6]=[C:7]([NH:17][C:18](=[O:25])OCC(Cl)(Cl)Cl)[N:8]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2].[NH2:26][C:27]1[C:28]([CH3:45])=[CH:29][C:30]([N:33]2[CH2:38][CH2:37][N:36]([C:39](=[O:44])[C:40]([CH3:43])([CH3:42])[CH3:41])[CH2:35][CH2:34]2)=[N:31][CH:32]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:1]([C:5]1[CH:6]=[C:7]([NH:17][C:18]([NH:26][C:27]2[CH:32]=[N:31][C:30]([N:33]3[CH2:34][CH2:35][N:36]([C:39](=[O:44])[C:40]([CH3:42])([CH3:41])[CH3:43])[CH2:37][CH2:38]3)=[CH:29][C:28]=2[CH3:45])=[O:25])[N:8]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)[N:9]=1)([CH3:3])([CH3:4])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 11430Potassium CarbonateHCID 99310942,2,2-Trichloroethyl 3-tert-butyl-1-P-tolyl-1H-pyrazol-5-ylcarbamateHCID 685380571-[4-(5-Amino-4-methyl-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one

생성물 1

HCID 68538008HCID 68538008, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

Add (5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-carbamic acid, 2,2,2-trichloro-ethyl ester (Preparation 38, 0.32 mmol, 0.1 r) over a solution of 1-[4-(5-amino-4-methyl-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one (0.3 mmol, 0.08 g) and potassium carbonate (0.3 mmol, 0.05 g) in acetonitrile (3 mL), and stir the solution for 4 hours at 80° C. Add water and extract with CH2Cl2. Combine the organic layers and wash with saturated aq. sodium chloride. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Subject residue to silica gel chromatography eluting with hexanes/ethyl acetate in gradient (from 20% to 80%). MS(ES+): m/z=532 [M+H].

후처리

  1. extractionAdd water and extract with CH2Cl2
  2. washwash with saturated aq. sodium chloride
  3. dry with materialDry over sodium sulfate
  4. filtrationfilter
  5. concentrationconcentrate under reduced pressure
  6. customto give a residue
  7. washSubject residue to silica gel chromatography eluting with hexanes/ethyl acetate in gradient (from 20% to 80%)

출처 및 근거

ORD 기록
ord-f617861c03ae450a81172f668c2e32e7
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652015B2

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