m-Chloroperbenzoic acid → 2-(2-Dimethylaminobenzylsulfinyl)quinoxaline

HRID 2107326노트

반응식

HRID 2107326 반응식
[CH3:1][N:2]([CH3:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][S:6][C:7]1[CH:16]=[N:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1.ClC1C=CC=C(C(OO)=[O:30])C=1>C(Cl)(Cl)Cl>[CH3:1][N:2]([CH3:21])[C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][S:6]([C:7]1[CH:16]=[N:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=1)=[O:30]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 140521762-(2-Dimethylaminobenzylthio)quinoxaline

생성물 1

HCID 140521812-(2-Dimethylaminobenzylsulfinyl)quinoxaline수율 21.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

In 50 ml of chloroform was dissolved 1.47 g of 2-(2-dimethylaminobenzylthio)quinoxaline. To the chilled solution kept at -10° C. was portionwise added 1.54 g of m-chloroperbenzoic acid (purity: 80%). To the reaction liquid were washed successively with saturated aqueous NaHCO3 solution, water and saturated aqueous sodium chloride solution, and dried over sodium sulfate. The sodium sulfate was then removed by filtration, and the solvent was evaporated under reduced pressure from the filtrate. The residue was purified by silica gel column chromatography (hexane/acetone) to give 330 mg of 2-(2-dimethylaminobenzylsulfinyl)quinoxaline as a yellow powder, m.p. 114°-115° C.

후처리

  1. customkept at -10° C.
  2. customTo the reaction liquid
  3. washwere washed successively with saturated aqueous NaHCO3 solution, water and saturated aqueous sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customThe sodium sulfate was then removed by filtration
  6. customthe solvent was evaporated under reduced pressure from the filtrate
  7. customThe residue was purified by silica gel column chromatography (hexane/acetone)

출처 및 근거

ORD 기록
ord-65639372115f4d2d8a329ec85f0b7150
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04933458

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