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m-Chloroperbenzoic acid → 2-(2-Diethylaminobenzylsulfinyl)-3-methylquinoxaline

HRID 2107331
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HRID 2107331 반응식
[CH2:1]([N:3]([CH2:23][CH3:24])[C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[CH2:6][S:7][C:8]1[C:17]([CH3:18])=[N:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1)[CH3:2].ClC1C=CC=C(C(OO)=[O:33])C=1>C(Cl)(Cl)Cl>[CH2:23]([N:3]([CH2:1][CH3:2])[C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[CH2:6][S:7]([C:8]1[C:17]([CH3:18])=[N:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1)=[O:33])[CH3:24]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 14052179HCID 14052179, 화합물

생성물 1

HCID 140521842-(2-Diethylaminobenzylsulfinyl)-3-methylquinoxaline수율 67.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

In 50 ml of chloroform was dissolved 1.7 g of 2-(2-diethylaminobenzylthio)-3-methylquinoxaline. To the chilled solution kept at -10° C. was portionwise added 1.21 g of m-chloroperbenzoic acid (purity: 80%). The reaction liquid was then 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 residual oil was purified by silica gel column chromatography (hexane/acetone) to give 1.2 g of 2-(2-diethylaminobenzylsulfinyl)-3-methylquinoxaline as a yellow oil.

후처리

  1. customkept at -10° C.
  2. customThe reaction liquid
  3. washwas then 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 residual oil was purified by silica gel column chromatography (hexane/acetone)

출처 및 근거

ORD 기록
ord-5f7b85b69d4f4c2e8674cd67d765d05d
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04933458

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