1-(4-Pyridyl)piperazine → HCID 18918480、化合物

HRID 864774ノート

反応式

HRID 864774 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12][S:13]([C:16]2[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=2)(=[O:15])=[O:14])=[CH:7][CH:6]=1)=[O:4].[N:23]1[CH:28]=[CH:27][C:26]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[CH:25][CH:24]=1>C(#N)C>[N:23]1[CH:28]=[CH:27][C:26]([N:29]2[CH2:30][CH2:31][N:32]([CH2:2][C:3]([C:5]3[CH:10]=[CH:9][C:8]([CH2:11][NH:12][S:13]([C:16]4[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=4)(=[O:15])=[O:14])=[CH:7][CH:6]=3)=[O:4])[CH2:33][CH2:34]2)=[CH:25][CH:24]=1

参加物

4

反応物 2

HCID 705171-(4-Pyridyl)piperazineHCID 18918612HCID 18918612、化合物

生成物 1

HCID 18918480HCID 18918480、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

A solution of N-([4-bromoacetylphenyl]methyl)-4-methylphenylsulphonamide (470 mg) in acetonitrile (10 ml) was added to a stirred solution of 1-(4-pyridyl)piperazine (400 mg) in acetonitrile (10 ml) and the mixture stirred for 18 hours. The solvent was evaporated in vacuo and the residue purified by flash chromatography on silica, eluting with 10% v/v methanol/dichloromethane. On evaporation of the eluant fraction to a small volume crystallisation occurred. These crystals, on filtration and washing with dichloromethane gave the title compound, 130 mg, as a solid: m.p. 215°-219° C. dec.; NMR(d6DMSO) δ8.14(3H,m), 7.91(2H,d), 7.69(2H,d), 7.38(4H,d), 6.82(2H,d), 4.03(2H,d), 3.89(2H,s), 3.32(4H,t), 2.62(4H,t), 2.39(3H,s); m/e 465(M+H)+ ; calculated for C25H28N4O3S: C, 64.6; N, 6.1; N, 12.1. found C, 64.7; H, 6.2; N, 12.0%.

後処理

  1. customThe solvent was evaporated in vacuo
  2. customthe residue purified by flash chromatography on silica
  3. washeluting with 10% v/v methanol/dichloromethane
  4. customOn evaporation of the eluant fraction
  5. customto a small volume crystallisation
  6. filtrationThese crystals, on filtration
  7. washwashing with dichloromethane

出典と根拠

ORDレコード
ord-ddd89a75cd6447f3ba101bd9c987cf7e
出典データセット
uspto-grants-1996_10
特許番号
US05563141

反応ノート

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