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Water → 2-[5-(4-chloro-phenyl)-1-(2,4-dichloro-phenyl)-4-ethyl-1H-pyrazol-3-yl]-3-methyl-3,5-dihydro-imidazol-4-one

HRID 1805207
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HRID 1805207 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]3[NH:25][C:24](=[O:26])[CH2:23][N:22]=3)[C:9]=2[CH2:27][CH3:28])=[CH:4][CH:3]=1.[C:29](=O)([O-])[O-].[K+].[K+].CI.O>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]3[N:25]([CH3:29])[C:24](=[O:26])[CH2:23][N:22]=3)[C:9]=2[CH2:27][CH3:28])=[CH:4][CH:3]=1
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6

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HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 593171472-[5-(4-chloro-phenyl)-1-(2,4-dichloro-phenyl)-4-ethyl-1H-pyrazol-3-yl]-3,5-dihydro-imidazol-4-one

생성물 1

HCID 593171542-[5-(4-chloro-phenyl)-1-(2,4-dichloro-phenyl)-4-ethyl-1H-pyrazol-3-yl]-3-methyl-3,5-dihydro-imidazol-4-one수율 68%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

To a solution of 26 (100 mg, 0.23 mmol) in acetonitrile (8 mL) at room temperature was sequentially added potassium carbonate (150 mg, 1.09 mole) and methyl iodide (2 g, 14.08 mmol) slowly. The mixture was stirred at 60° C. for 6 h. Water was added and the resulting mixture was extracted with ethyl acetate (2×50 mL). The combined extracts were washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. Purification of the crude residue by flash chromatography on silica gel eluting with hexanes/ethyl acetate (1:1) gave the compound 29 (70 mg, 68%) as a white solid. 1H NMR (400 MHz, CDCl3) δ 7.45 (d, 1H), 7.30 (d, 2H), 7.25 (dd, 1H), 7.18 (d, 1H), 7.09 (d, 2H), 4.88 (s, 0.82H), 4.51 (s, 1.18H), 3.42 (s, 1.77H), 3.24 (s, 1.23H), 2.65 (q, 2H), 1.15 (t, 3H); ESMS m/: 447.0 (M+1).

후처리

  1. customat room temperature
  2. extractionthe resulting mixture was extracted with ethyl acetate (2×50 mL)
  3. washThe combined extracts were washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification of the crude residue by flash chromatography on silica gel eluting with hexanes/ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-e55db8be060c464aa726e69ec4990574
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08354442B2

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