1-(4-Pyridyl)piperazine → HCID 18918516, 화합물

HRID 864776노트

반응식

HRID 864776 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][S:14]([C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)(=[O:16])=[O:15])=[CH:7][CH:6]=1)=[O:4].[N:24]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]2)=[CH:26][CH:25]=1>C(#N)C>[N:24]1[CH:29]=[CH:28][C:27]([N:30]2[CH2:31][CH2:32][N:33]([CH2:2][C:3]([C:5]3[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][S:14]([C:17]4[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=4)(=[O:16])=[O:15])=[CH:7][CH:6]=3)=[O:4])[CH2:34][CH2:35]2)=[CH:26][CH:25]=1

참가 물질

4

반응물 2

HCID 705171-(4-Pyridyl)piperazineHCID 18918520HCID 18918520, 화합물

생성물 1

HCID 18918516HCID 18918516, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of N-(2-[4-bromoacetylphenyl]ethyl)-4-methylphenylsulphonamide (485 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 was 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 crystallisation occured. These crystals on filtration and washing with dichloromethane gave the title compound, 230 mg, as an off-white solid: m.p. 133°-135° C.; NMR(d6DMSO) δ8.14(2H,bd), 7.90(2H,d), 7.65(2H,d), 7.59(1H,t), 7.35(2H,d), 7.29(2H,d), 6.81(2H,d), 3.37(2H,s), 3.33(4H,t), 2.98(2H,q), 2.76(2H,t), 2.63(4H,t), 2.38(3H,s); m/e 479(M+H)+ ; calculated for C26H30N4O3S: C, 65.2; H, 6.3; N, 11.7; found. C 65.0; H, 6.3; N, 11.4%.

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 crystallisation
  5. filtrationThese crystals on filtration
  6. washwashing with dichloromethane

출처 및 근거

ORD 기록
ord-91945c4fea3a4e539b368eb8f8e7aa2d
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05563141

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