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Methanesulfonyl chloride → HCID 178477812, 화합물

HRID 1506224
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HRID 1506224 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[N:11]=[CH:10][NH:9][C:5]2=[N+:6]([O-])[CH:7]=1.CS([Cl:16])(=O)=O.C(=O)([O-])O.[Na+]>CN(C)C=O>[Br:1][C:2]1[C:3]([Cl:16])=[C:4]2[N:11]=[CH:10][NH:9][C:5]2=[N:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 178526232HCID 178526232, 화합물

생성물 1

HCID 178477812HCID 178477812, 화합물수율 52.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
73 °C

실험 절차

6-Bromo-3H-imidazo[4,5-b]pyridine 4-oxide (1.88 g, 8.82 mmol) in N,N-dimethylformamide (12 mL) was heated to 50° C., mixed with methansulfonyl chloride (8.00 mL, 103 mmol) and stirred at 73° C. for 3 hours. The reaction mixture was cooled with ice and gradually poured into saturated aqueous sodium hydrogen carbonate (75 mL), and the precipitated solid was collected by filtration, washed with water and chloroform and dried under reduced pressure to give the title compound as a dark brown solid (1.07 g, yield 52%).

후처리

  1. temperatureThe reaction mixture was cooled with ice
  2. filtrationthe precipitated solid was collected by filtration
  3. washwashed with water and chloroform
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-99b09c1769904fb2808fc4a13284a878
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216999B2

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