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Acetic Acid → 2,3-dichloro-N-{3-chloroquinoxalin-2-yl}benzenesulfonamide

HRID 1186310
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HRID 1186310 반응식
Cl[C:2]1[C:11]([Cl:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[Cl:13][C:14]1[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=1[S:21]([NH2:24])(=[O:23])=[O:22].C(=O)([O-])[O-].[K+].[K+].C(O)(=O)C>CS(C)=O>[Cl:13][C:14]1[C:19]([Cl:20])=[CH:18][CH:17]=[CH:16][C:15]=1[S:21]([NH:24][C:2]1[C:11]([Cl:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1)(=[O:22])=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 11430Potassium CarbonateHCID 166592,3-DichloroquinoxalineHCID 83179472,3-Dichlorobenzenesulfonamide

생성물 1

HCID 866579282,3-dichloro-N-{3-chloroquinoxalin-2-yl}benzenesulfonamide수율 78.4%

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

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온도
150 °C

실험 절차

2,3-Dichloroquinoxaline (1.00 g, 5.02 mmol), 2,3-dichlorobenzenesulfonamide (1.41 g, 5.02 mmol) and potassium carbonate (694 mg, 5.02 mmol) were suspended in dimethyl sulfoxide (30 mL) and the mixture was stirred at 150° C. for 3 hours. The reaction mixture was slowly added to a mixture (300 ml) of a 1% aqueous acetic acid solution and ice, and the mixture was stirred for 3 hours. The resulting solid was collected by filtration and washed with water. Then, slurry purification was performed using diisopropyl ether, to give 2,3-dichloro-N-{3-chloroquinoxalin-2-yl}benzenesulfonamide (Compound AA) (1.53 g, yield: 78%).

후처리

  1. stirringthe mixture was stirred for 3 hours
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with water
  4. customThen, slurry purification

출처 및 근거

ORD 기록
ord-0ee91c783d064b49b046d9c432bcd921
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673908B2

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