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Pyridine → N-[4-chloro-2-(2-chlorobenzyl)phenyl]-3-methoxybenzenesulfonamide

HRID 747611
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인쇄 미리보기

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HRID 747611 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Cl:16])[CH:3]=1.N1C=CC=CC=1.[CH3:23][O:24][C:25]1[CH:26]=[C:27]([S:31](Cl)(=[O:33])=[O:32])[CH:28]=[CH:29][CH:30]=1>C1COCC1.C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][S:31]([C:27]2[CH:28]=[CH:29][CH:30]=[C:25]([O:24][CH3:23])[CH:26]=2)(=[O:33])=[O:32])=[C:4]([CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[Cl:16])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1049PyridineHCID 27375043-Methoxybenzenesulfonyl chlorideHCID 143578744-Chloro-2-[(2-chlorophenyl)methyl]aniline

생성물 1

HCID 68565360N-[4-chloro-2-(2-chlorobenzyl)phenyl]-3-methoxybenzenesulfonamide수율 56%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

Starting with 0.71 g of [4-chloro-2-(2-chlorobenzyl)phenyl]amine dissolved in 5 ml of THF are added 0.4 ml of pyridine and 0.8 g of 3-methoxybenzenesulfonyl chloride, and the mixture is left at room temperature for 18 hours. The reaction medium is taken up in ethyl acetate and washed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is chromatographed on a column of silica gel, eluting with a 90/10 (v/v) cyclohexane/ethyl acetate solvent mixture to give 0.666 g of expected product.

후처리

  1. washwashed with water
  2. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe residue is chromatographed on a column of silica gel
  5. washeluting with a 90/10 (v/v) cyclohexane/ethyl acetate solvent mixture

출처 및 근거

ORD 기록
ord-3c9ab68c341247d0b0b236e22bf92e09
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07396958B2

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