Acetic Acid → HCID 12276122, 화합물

HRID 428145

반응식

HRID 428145 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 12276122HCID 12276122, 화합물수율 60.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-0fe0dd5283cf4905b42ee79271a7a6cb
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313153B1

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