4-(5-Bromo-3-methyl-2-pyridinyl)butylamine → 2-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine

HRID 1607033

反応式

HRID 1607033 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH3:13])[C:5]([CH2:8][CH2:9][CH2:10][CH2:11][NH2:12])=[N:6][CH:7]=1.Cl.Cl[C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:19]([CH2:25][C:26]2[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=2)=[CH:18][N:17]=1>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH3:13])[C:5]([CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:16]2[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:19]([CH2:25][C:26]3[CH:27]=[N:28][CH:29]=[CH:30][CH:31]=3)=[CH:18][N:17]=2)=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 130942724-(5-Bromo-3-methyl-2-pyridinyl)butylamineHCID 198517872-Chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride

生成物 1

HCID 198517932-[4-(5-Bromo-3-methylpyrid-2-yl)butylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-(5-bromo-3-methylpyrid-2-yl)butylamine (11.79 g) and 2-chloro-3-nitro-5-(pyrid-3-ylmethyl)-pyridine hydrochloride (4.57 g) was refluxed in ethanol (100 ml) for 8 hours. The solvent was removed in vacuo, the residue was dissolved in water (100 ml) and then extracted with chloroform (100 ml). The chloroform extract was chromatographed on silica eluted with 5% v/v methanol in chloroform followed by recrystallisation from chloroform/hexane to give the title compound as a yellow solid, m.p. 82°-84° C.

後処理

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in water (100 ml)
  3. extractionextracted with chloroform (100 ml)
  4. extractionThe chloroform extract
  5. customwas chromatographed on silica
  6. washeluted with 5% v/v methanol in chloroform
  7. customfollowed by recrystallisation from chloroform/hexane

出典と根拠

ORDレコード
ord-bfab609de5ad49b8aabcf0db1a4e32d6
出典データセット
uspto-grants-1989_09
特許番号
US04863933

関連ノート

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