Acetic Acid → HCID 12276122、化合物

HRID 428145

反応式

HRID 428145 の反応式
[CH3:1][S-:2].[Na+].[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH:14]=[CH:15][C:16]=1[O:17][CH3:18])/[CH:9]=[CH:10]/[N+:11]([O-:13])=[O:12].C(O)(=O)C>CO>[CH3:4][O:5][C:6]1[CH:7]=[C:8]([CH:9]([S:2][CH3:1])[CH2:10][N+:11]([O-:13])=[O:12])[CH:14]=[CH:15][C:16]=1[O:17][CH3:18]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 7096881,2-Dimethoxy-4-(2-nitrovinyl)benzeneHCID 4378561Sodium methanethiolate

生成物 1

HCID 12276122HCID 12276122、化合物収率 60.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of sodium methanethiolate (0.62 g, 8.8 mmol) in methanol (20 ml), trans-3,4-dimethoxy-β-nitrostyrene (1.42 g, 8 mmol) was added and stirred at room temperature for 5 minutes. Further, acetic acid (0.46 ml) was added and stirred for 5 minutes. After evaporating methanol to a half amount under reduced pressure, water was added and extracted with dichloromethane and the organic layers were combined, washed with water and dried over sodium sulfate. The solvent was distilled out under reduced pressure and the residue was isolated and purified by silica gel column chromatography (hexane:ethyl acetate=10:1) to yield 2-(3,4-dimethoxyphenyl)-2-(methylthio)nitroethane (1.24 g, 60%).

後処理

  1. stirringstirred for 5 minutes
  2. customAfter evaporating methanol to a half amount under reduced pressure, water
  3. additionwas added
  4. extractionextracted with dichloromethane
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. distillationThe solvent was distilled out under reduced pressure
  8. customthe residue was isolated
  9. custompurified by silica gel column chromatography (hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-0fe0dd5283cf4905b42ee79271a7a6cb
出典データセット
uspto-grants-2001_11
特許番号
US06313153B1

関連ノート

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