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Hydrochloric Acid → N-(4-methylsulfonylphenylsulfonyl)-2-chloroisonicotinamide

HRID 2308611
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HRID 2308611 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]=[CH:23][N:24]=1)[C:19](Cl)=[O:20].Cl.CCCCCC.C(OCC)(=O)C>N1C=CC=CC=1>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([S:11]([NH:14][C:19](=[O:20])[C:18]2[CH:22]=[CH:23][N:24]=[C:16]([Cl:15])[CH:17]=2)(=[O:13])=[O:12])=[CH:9][CH:10]=1)(=[O:4])=[O:3]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1203134-(Methanesulfonyl)benzene-1-sulfonamideHCID 28000032-Chloropyridine-4-carbonyl chlorideHCID 21226206Ethyl acetate hexane

생성물 1

HCID 13924304N-(4-methylsulfonylphenylsulfonyl)-2-chloroisonicotinamide수율 74.7%

시약·촉매·용매 1

HCID 1049
Pyridine
용매

실험 절차

2.3 g (0.01 mol) of 4-methylsulfonylbenzenesulfonamide were dissolved in 20 ml of pyridine, and added dropwise by 1.7 g (0.01 mol) of 2-chloroisonicotinoyl chloride at room temperature, followed by agitation for 2 hrs. at the same temperature. After acidified by adding aqueous hydrochloric acid, the precipitate was extracted by ethyl acetate. The organic layer obtained was dried and then concentrated to precipitate crude crystals, which were recrystallized by n-hexane/ethyl acetate to 2.8 g (yield: 74.7%) of N-(4-methylsulfonylphenylsulfonyl)-2-chloroisonicotinamide as white crystals.

후처리

  1. extractionthe precipitate was extracted by ethyl acetate
  2. customThe organic layer obtained
  3. customwas dried
  4. concentrationconcentrated
  5. customto precipitate crude crystals, which

출처 및 근거

ORD 기록
ord-e97899d99d384486be14ddeb173e2a60
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04690934

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