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

HRID 2107326ノート

反応式

HRID 2107326 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 140521812-(2-Dimethylaminobenzylsulfinyl)quinoxaline収率 21.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-65639372115f4d2d8a329ec85f0b7150
出典データセット
uspto-grants-1990_06
特許番号
US04933458

反応ノート

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