Potassium Iodide → 2-Amino-3-(2-methylbenzylamino)pyrazine

HRID 4294

反応式

HRID 4294 の反応式
[NH2:1][C:2]1[C:7](Cl)=[N:6][CH:5]=[CH:4][N:3]=1.[CH3:9][C:10]1[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=1[CH2:12][NH2:13].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.O>[NH2:1][C:2]1[C:7]([NH:13][CH2:12][C:11]2[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=2[CH3:9])=[N:6][CH:5]=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 69932-MethylbenzylamineHCID 11430Potassium CarbonateHCID 2762242-Amino-3-chloropyrazine

生成物 1

HCID 201523282-Amino-3-(2-methylbenzylamino)pyrazine収率 19.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-amino-3-chloropyrazine (4.3 g), 2-methylbenzylamine (4.6 g), potassium carbonate (5.5 g), and potassium iodide (0.4 g) in N,N-dimethylformamide (43 ml) was refluxed for 24 hours under a nitrogen atmosphere and allowed to stand at room temperature. The mixture was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent to give 2-amino-3-(2-methylbenzylamino)pyrazine (1.4 g).

後処理

  1. temperaturewas refluxed for 24 hours under a nitrogen atmosphere
  2. customto stand at room temperature
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent

出典と根拠

ORDレコード
ord-9d28aa19805e4a3182693ceb169ad3c2
出典データセット
uspto-grants-1988_02
特許番号
US04725601

関連ノート

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