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2-Nitroamino-5-(2-methoxy-4-pyridyl)methyl-4-pyrimidone → 2-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamino-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone

HRID 1904082
ノート
印刷プレビュー

反応式

HRID 1904082 の反応式
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12][CH2:13][CH2:14][NH2:15])[CH:6]=1)[CH3:3].[N+](N[C:20]1[NH:25][C:24](=[O:26])[C:23]([CH2:27][C:28]2[CH:33]=[CH:32][N:31]=[C:30]([O:34][CH3:35])[CH:29]=2)=[CH:22][N:21]=1)([O-])=O>N1C=CC=CC=1>[CH3:3][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12][CH2:13][CH2:14][NH:15][C:20]2[NH:25][C:24](=[O:26])[C:23]([CH2:27][C:28]3[CH:33]=[CH:32][N:31]=[C:30]([O:34][CH3:35])[CH:29]=3)=[CH:22][N:21]=2)[CH:6]=1)[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 127838332-Nitroamino-5-(2-methoxy-4-pyridyl)methyl-4-pyrimidoneHCID 132773272-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamine

生成物 1

HCID 132926052-(4-Dimethylaminomethyl-2-pyridylmethylthio)ethylamino-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone収率 61.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (1 g) and 2-nitroamino-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone (1.23 g) was refluxed in pyridine (6 ml) for 10 hours, concentrated in vacuo and chromatographed on silica gel column eluted with ethyl acetate-ethanol-28% W:W aqueous ammonia (by volume 10:15:2). Recrystallisation from acetonitrile:ether (1:5) gave 2-[2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamino-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone (1.21 g) m.p. 65°-74° C.

後処理

  1. concentrationconcentrated in vacuo
  2. customchromatographed on silica gel column
  3. washeluted with ethyl acetate-ethanol-28% W
  4. customRecrystallisation from acetonitrile:ether (1:5)

出典と根拠

ORDレコード
ord-d953307ca22c460aacf3d4ff8f3c4ca8
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04439609

反応ノート

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