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Hydrochloric Acid → HCID 59410236, 화합물

HRID 1891383
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HRID 1891383 반응식
[Cl:1][C:2]1[C:7]([C:8]2[CH:9]=[N:10][C:11]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:13]=2[C:14]#[N:15])=[CH:6][C:5]([S:20](Cl)(=[O:22])=[O:21])=[C:4]([O:24][CH3:25])[CH:3]=1.N1C=CC=CC=1.[CH3:32][NH:33][C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.Cl>ClCCl>[Cl:1][C:2]1[C:7]([C:8]2[CH:9]=[N:10][C:11]([C:16]([F:19])([F:18])[F:17])=[CH:12][C:13]=2[C:14]#[N:15])=[CH:6][C:5]([S:20]([N:33]([CH3:32])[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)(=[O:22])=[O:21])=[C:4]([O:24][CH3:25])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 7515N-MethylanilineHCID 866435054-Chloro-5-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-2-methoxy-benzenesulfonyl chloride

생성물 1

HCID 59410236HCID 59410236, 화합물수율 93.4%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To 4-chloro-5-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-2-methoxy-benzenesulfonyl chloride (100 mg, 0.24 mmol) in dichloromethane (3 mL), was added pyridine (0.04 mL, 0.48 mmol), followed by addition of N-methylaniline (0.05 mL, 0.48 mmol). The mixture was stirred at r.t. for 16 hrs, then poured into 1 N HCl solution (10 mL). The product was extracted with ethyl acetate and the organic layer was washed with 1N HCl and water, then was dried over MgSO4. Concentration gave 4-chloro-5-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-2-methoxy-N-methyl-N-phenyl-benzenesulfonamide 15-1, (108 mg). MS: 482.0 (M+H)+; tR=8.76 min (method 2).

후처리

  1. extractionThe product was extracted with ethyl acetate
  2. washthe organic layer was washed with 1N HCl and water
  3. dry with materialwas dried over MgSO4
  4. concentrationConcentration

출처 및 근거

ORD 기록
ord-af87f2edf19c4afc9ed4888389c84eaa
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507536B2

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