P-Toluenesulfonamide → N-[4-[4-(3,4-Dichlorophenoxy)-1-piperidinyl]-1-oxobutyl]-4-methyl-benzenesulfonamide

HRID 915548ノート

反応式

HRID 915548 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[Cl:22])[O:6][CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][C:16]([OH:18])=O)[CH2:9][CH2:8]1.[CH3:23][C:24]1[CH:25]=[CH:26][C:27]([S:30]([NH2:33])(=[O:32])=[O:31])=[CH:28][CH:29]=1.CN(C1C=CC=CN=1)C.CCN=C=NCCCN(C)C>ClCCl>[Cl:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[Cl:22])[O:6][CH:7]1[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][C:16]([NH:33][S:30]([C:27]2[CH:28]=[CH:29][C:24]([CH3:23])=[CH:25][CH:26]=2)(=[O:31])=[O:32])=[O:18])[CH2:11][CH2:12]1

参加物

6

反応物 4

HCID 6269P-ToluenesulfonamideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 218852-DimethylaminopyridineHCID 694203114-(3,4-Dichlorophenoxy)-1-piperidinebutanoic acid hydrochloride

生成物 1

HCID 69418750N-[4-[4-(3,4-Dichlorophenoxy)-1-piperidinyl]-1-oxobutyl]-4-methyl-benzenesulfonamide収率 12.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-(3,4-Dichlorophenoxy)-1-piperidinebutanoic acid hydrochloride (0.250 g) was dissolved in dichloromethane (10 mL) containing p-toluenesulfonamide (0.142 g), dimethylaminopyridine (92 mg) and EDCI (0.158 g) were added. The solution was stirred at room temperature for 4 days. The solvent was evaporated. The crude product was dried in vacuo and then purified by HPLC (at column dilution, gradient ammonium acetate/acetonitrile 75% to 5% ;Waters Xterra® column) and to give the title compound (42 mg).

後処理

  1. additionwere added
  2. customThe solvent was evaporated
  3. dry with materialThe crude product was dried in vacuo
  4. custompurified by HPLC (at column dilution, gradient ammonium acetate/acetonitrile 75% to 5% ;Waters Xterra® column)

出典と根拠

ORDレコード
ord-78a1118f2fe149669a35b69e2a69d9a9
出典データセット
uspto-grants-2007_09
特許番号
US07265227B2

反応ノート

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