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

HRID 1030797
ノート
印刷プレビュー

反応式

HRID 1030797 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 14052179HCID 14052179、化合物

生成物 1

HCID 140521842-(2-Diethylaminobenzylsulfinyl)-3-methylquinoxaline収率 67.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-fc65e368786043f2a5d24b9e0075991b
出典データセット
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05106976

反応ノート

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