Methyl iodide → HCID 20396007, 화합물

HRID 261061노트

반응식

HRID 261061 반응식
[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][NH:11][C:10](=[O:14])[CH2:9]2)[CH:5]=[N:4][CH:3]=1.[H-].[Na+].[CH3:17]I>CN(C)C=O.C1(C)C=CC=CC=1.O>[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH3:17])[C:10](=[O:14])[CH2:9]2)[CH:5]=[N:4][CH:3]=1

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 203960024-(6-Chloropyrazin-2-yl)piperazin-2-one

생성물 1

HCID 20396007HCID 20396007, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

The product of Example 1 (2.13 g, 0.01 mole) and sodium hydride-oil suspension (50%, 0.50 g, 0.01 mole) are combined in 10 ml N,N-dimethylformamide and the stirred mixture treated with 0.65 ml (0.01 mole) of methyl iodide in 5 ml toluene. The mixture is stirred 1 hour at room temperature, diluted with water and extracted with toluene. The toluene extracts are washed with water, dried over sodium sulfate, filtered and concentrated in vacuo to give the crude product which is chromatographed on neutral (activity III) alumina. Elution with chloroform gives fractions containing 1.4 of a white solid which is recrystallized from n-butylchloride-cyclohexane to give white crystals of the title compound, mp 122°-123° C.

후처리

  1. extractionextracted with toluene
  2. washThe toluene extracts are washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give the crude product which
  7. customis chromatographed on neutral (activity III) alumina
  8. washElution with chloroform
  9. customgives fractions
  10. additioncontaining 1.4 of a white solid which
  11. customis recrystallized from n-butylchloride-cyclohexane

출처 및 근거

ORD 기록
ord-a15cf56d07ab40e8b21ff65fc97f3d36
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04163849

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