Water → HCID 178527559, 화합물

HRID 1740997

반응식

HRID 1740997 반응식
[NH2:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:5]([S:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[CH:16]=2)[NH:4][N:3]=1.[Cl:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[S:37](Cl)(=[O:39])=[O:38].O>N1C=CC=CC=1>[Cl:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[S:37]([NH:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:5]([S:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:23]=[CH:24][C:25]([F:28])=[CH:26][CH:27]=3)[CH:16]=2)[NH:4][N:3]=1)(=[O:39])=[O:38]

참가 물질

5

반응물 3

HCID 962WaterHCID 5221832,6-DichlorobenzenesulfonylchlorideHCID 178509293HCID 178509293, 화합물

생성물 1

HCID 178527559HCID 178527559, 화합물수율 53.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3-Amino-4-(2-pyridyl)-5-(3-(4-fluorophenoxy)benzylthio)-(1H)-pyrazole (0.39 g, 0.99 mmol) was dissolved in 5 ml of pyridine. Commercial 2,6-dichlorobenzenesulfonyl chloride (0.26 g, 1.04 mmol) was added and the red solution was stirred overnight at room temperature. The reaction mixture was poured into 50 ml of water and was extracted twice with 100 ml portions of ethyl acetate. The organic layers were washed with water and brine, combined, dried over MgSO4 and concentrated. The crude product was slurried in cold ethyl acetate and the solid was filtered off and washed with small portions of cold ethyl acetate and cold diethyl ether and dried under vacuum to afford 0.32 g (53% yield) of the final compound.

후처리

  1. extractionwas extracted twice with 100 ml portions of ethyl acetate
  2. washThe organic layers were washed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. filtrationthe solid was filtered off
  6. washwashed with small portions of cold ethyl acetate and cold diethyl ether
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-f41f426eeca54d00ae9fbc53b55e4f30
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972972

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