Methane, dichloromethoxy- → 5-Chloro-2-methoxy-3-methylbenzaldehyde

HRID 2290537ノート

反応式

HRID 2290537 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[O:9]C.[CH3:11][O:12][CH:13](Cl)Cl>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[Cl:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:13]([O:12][CH3:11])=[C:4]([CH:5]=1)[CH:3]=[O:9]

参加物

5

反応物 2

HCID 21004Methane, dichloromethoxy-HCID 767484-Chloro-2-methylanisole

生成物 1

HCID 133167535-Chloro-2-methoxy-3-methylbenzaldehyde

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Titanium tetrachloride (21.6 g, 0.114 mole) was added to a solution of 2-methyl-4-chloroanisole (9 g, 0.057 mole) in methylene chloride at 0° C. Then, 1,1-dichloromethyl methyl ether (7.24 g, 0.063 mole) was added dropwise over a three minute period and the reaction mixture stirred at 0° C. for 30 minutes. The reaction was quenched by carefully pouring it into water (600 ml). The organic layer was separated and the aqueous phase extracted with methylene chloride (2×100 ml). The combined organic layer and extracts was washed with brine, dried (MgSO4) and concentrated under reduced pressure to a pale yellow solid (10.1 g).

後処理

  1. customThe reaction was quenched
  2. additionby carefully pouring it into water (600 ml)
  3. customThe organic layer was separated
  4. extractionthe aqueous phase extracted with methylene chloride (2×100 ml)
  5. washThe combined organic layer and extracts was washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure to a pale yellow solid (10.1 g)

出典と根拠

ORDレコード
ord-d70ad4294ed1496f811f32daceee59ea
出典データセット
uspto-grants-1986_10
特許番号
US04617312

反応ノート

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