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

HRID 915548노트

반응식

HRID 915548 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-78a1118f2fe149669a35b69e2a69d9a9
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265227B2

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