Methane, dichloromethoxy- → HCID 12629035, 화합물

HRID 1743382노트

반응식

HRID 1743382 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[C:5]([CH3:11])[C:4]=1[CH3:12].[CH3:13][O:14]C(Cl)Cl>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[CH3:10][O:9][C:6]1[C:5]([CH3:11])=[C:4]([CH3:12])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[CH:13]=[O:14]

참가 물질

5

반응물 2

HCID 21004Methane, dichloromethoxy-HCID 148299Benzene, 1,4-dimethoxy-2,3-dimethyl-

생성물 1

HCID 12629035HCID 12629035, 화합물수율 92%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1,4-dimethoxy-2,3-dimethylbenzene (100 g, 0.60 mol) and dichloromethyl methyl ether (65 mL, 0.72 mol) in dichloromethane (400 mL) was added dropwise titanium tetrachloride (IV)(100 mL, 0.91 mol) over 30 minutes under ice-cooling, and the mixture was stirred at the same temperature for 30 minutes. The reaction mixture was poured into ice (1 kg), the organic layer was separated, and the aqueous layer was extracted twice with dichloromethane. The combined organic layers were washes with water and saturated brine, passed through sodium sulfate-silica gel, dried (eluted with hexane-ethyl acetate 5:1) and concentrated under reduced pressure. The residue was recrystallized from hexane to obtain 107 g of the title compound.

후처리

  1. temperaturecooling
  2. customthe organic layer was separated
  3. extractionthe aqueous layer was extracted twice with dichloromethane
  4. customdried
  5. wash(eluted with hexane-ethyl acetate 5:1)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from hexane

출처 및 근거

ORD 기록
ord-d8753d3c3fb2443b9f7096f86d374306
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07008940B1

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