Methyl iodide → HCID 20396007、化合物

HRID 261061ノート

反応式

HRID 261061 の反応式
[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

参加物

7

反応物 3

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

生成物 1

HCID 20396007HCID 20396007、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a15cf56d07ab40e8b21ff65fc97f3d36
出典データセット
uspto-grants-1979_08
特許番号
US04163849

反応ノート

読み込み中…