Triethylamine → 3-(5,6,7,8-Tetrahydroquinol-8-yl)propylamino-3-nitro-5-(pyrid-3-ylmethyl)pyridine

HRID 1607039

반응식

HRID 1607039 반응식
[N:1]1[C:10]2[CH:9]([CH2:11][CH2:12][CH2:13][NH2:14])[CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.Cl[C:17]1[C:22]([N+:23]([O-:25])=[O:24])=[CH:21][C:20]([CH2:26][C:27]2[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=2)=[CH:19][N:18]=1.C(N(CC)CC)C>C(O)C>[N:1]1[C:10]2[CH:9]([CH2:11][CH2:12][CH2:13][NH:14][C:17]3[C:22]([N+:23]([O-:25])=[O:24])=[CH:21][C:20]([CH2:26][C:27]4[CH:28]=[N:29][CH:30]=[CH:31][CH:32]=4)=[CH:19][N:18]=3)[CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 198517793-(5,6,7,8-Tetrahydroquinol-8-yl)propylamineHCID 198517872-Chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride

생성물 1

HCID 198517973-(5,6,7,8-Tetrahydroquinol-8-yl)propylamino-3-nitro-5-(pyrid-3-ylmethyl)pyridine수율 86.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 3-(5,6,7,8-tetrahydroquinol-8-yl)-propylamine (4.5 g), 2-chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride (5 g) and triethylamine (10 ml) was refluxed in ethanol (200 ml) for 7.5 hours. The solvent was removed in vacuo, the residue was dissolved in chloroform and chromatographed on silica in chloroform and later chloroform/methanol 4:1. The fractions containing the product were concentrated to give the title compound as an oil (6.1 g).

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in chloroform
  3. customchromatographed on silica in chloroform and later chloroform/methanol 4:1
  4. additionThe fractions containing the product
  5. concentrationwere concentrated

출처 및 근거

ORD 기록
ord-42c680ba277747ad9aa03c0179e61677
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863933

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