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m-Chloroperbenzoic acid → HCID 86689846, 화합물

HRID 2409031
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HRID 2409031 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[N:10]([S:11]([C:14]3[CH:20]=[CH:19][C:17]([CH3:18])=[CH:16][CH:15]=3)(=[O:13])=[O:12])[CH:9]=[CH:8][C:5]2=[N:6][CH:7]=1.ClC1C=CC=C(C(OO)=[O:29])C=1>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]2[N:10]([S:11]([C:14]3[CH:20]=[CH:19][C:17]([CH3:18])=[CH:16][CH:15]=3)(=[O:13])=[O:12])[CH:9]=[CH:8][C:5]2=[N+:6]([O-:29])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 86689845HCID 86689845, 화합물

생성물 1

HCID 86689846HCID 86689846, 화합물수율 97.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 6-chloro-1-tosyl-1H-pyrrolo[3,2-b]pyridine (8.5 g, 27.7 mmol) in CH2Cl2 (150 mL) in an ice bath was added m-chloroperbenzoic acid (85%, 8.4 g, 41.6 mmol). The mixture was stirred at RT for two h. The reaction mixture was quenched by saturated sodium thiosulphate solution. The organic layer was washed with saturated NaHCO3 solution and water, dried (Na2SO4) filtered, and concentrated under reduced pressure to afford 8.75 g (90%) of 6-chloro-1-tosyl-1H-pyrrolo[3,2-b]pyridine-4-oxide as a yellow solid. MS (ESI): m/z=323.0 [M+1]+.

후처리

  1. customThe reaction mixture was quenched by saturated sodium thiosulphate solution
  2. washThe organic layer was washed with saturated NaHCO3 solution and water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d1bf975ec82f4b599bac37524b31d091
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08815877B2

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