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

반응식

HRID 1607033 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bfab609de5ad49b8aabcf0db1a4e32d6
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863933

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