1-(4-Pyridyl)piperazine → HCID 18918480, 화합물

HRID 864774노트

반응식

HRID 864774 반응식
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

참가 물질

4

반응물 2

HCID 705171-(4-Pyridyl)piperazineHCID 18918612HCID 18918612, 화합물

생성물 1

HCID 18918480HCID 18918480, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-ddd89a75cd6447f3ba101bd9c987cf7e
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05563141

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