Dichloromethane → 2-Chloro-3,4,5,6-tetramethoxybenzaldehyde

HRID 1527672

반응식

HRID 1527672 반응식
[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[C:8]([O:15][CH3:16])=[CH:7][C:4]=1[CH:5]=[O:6].C(Cl)[Cl:18]>>[Cl:18][C:7]1[C:8]([O:15][CH3:16])=[C:9]([O:13][CH3:14])[C:10]([O:11][CH3:12])=[C:3]([O:2][CH3:1])[C:4]=1[CH:5]=[O:6]

참가 물질

3

반응물 2

HCID 6344Dichloromethane2회HCID 6394122,3,4,5-Tetramethoxybenzaldehyde

생성물 1

HCID 461798872-Chloro-3,4,5,6-tetramethoxybenzaldehyde수율 97%

실험 절차

According to a general aryl chlorination procedure by Lopez-Alvarado,39 19 (0.767 g, 3.39 mmol) was dissolved in CH2Cl2 (10.0 mL) at room temperature and then SO2Cl2 (neat, 0.31 mL, 3.7 mmol) was added at room temperature. The reaction was stirred for 1 hour and monitored by 1H NMR for completion. The reaction was then diluted with CH2Cl2, washed with brine, dried over MgSO4, filtered, and condensed. The resulting oil was then purified by flash column chromatography (1:4 Et2O:hexanes) to provide 20 (0.861 g, 3.30 mmol, 97%) as a colorless oil.

후처리

  1. washwashed with brine
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customcondensed
  5. customThe resulting oil was then purified by flash column chromatography (1:4 Et2O:hexanes)

출처 및 근거

ORD 기록
ord-5c7bfab050e24190949009acdbd8cfe8
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09089605B2

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