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Sodium Carbonate → N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine

HRID 1085857
ノート
印刷プレビュー

反応式

HRID 1085857 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.Cl.Cl.[N:13]1[CH:18]=[CH:17][N:16]=[CH:15][C:14]=1[CH2:19][NH2:20].CN(C)C(=O)C.C(=O)([O-])[O-].[Na+].[Na+]>CC(C)CC(=O)C.O>[N+:8]([C:7]1[C:2]([NH:20][CH2:19][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][N:13]=2)=[N:3][CH:4]=[CH:5][CH:6]=1)([O-:10])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 31374DimethylacetamideHCID 796132-Chloro-3-nitropyridineHCID 19911503Pyrazin-2-ylmethanamine dihydrochloride

生成物 1

HCID 17845733N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine収率 10%

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 7909Methyl Isobutyl Ketone溶媒

反応条件

温度
100 °C

実験手順

To a stirred solution of 25.4 parts of 2-chloro-3-nitropyridine, 29.5 parts of 2-pyrazinemethanamine dihydrochloride and 235 parts of N,N-dimethylacetamide were added 67.8 parts of sodium carbonate. The reaction mixture was stirred for 1.5 hours at 100° C. The reaction mixture was poured into water and 4-methyl-2-pentanone. The whole was filtered twice over diatomaceous earth and the layers were separated. The organic layer was dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 3.6 parts (10%) of N-(3-nitro-2-pyridinyl)-2-pyrazinemethanamine (int. 27).

後処理

  1. filtrationThe whole was filtered twice over diatomaceous earth
  2. customthe layers were separated
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was crystallized from acetonitrile
  7. filtrationThe product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-935ac279230d4cb6af5a160072d62db6
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05011842

反応ノート

読み込み中…

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