Methane, dichloromethoxy- → HCID 12629035、化合物

HRID 1743382ノート

反応式

HRID 1743382 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 12629035HCID 12629035、化合物収率 92%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8753d3c3fb2443b9f7096f86d374306
出典データセット
uspto-grants-2006_03
特許番号
US07008940B1

反応ノート

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