Water → 4-Chloro-2-fluoro-5-methoxybenzyl chloride

HRID 1003989ノート

反応式

HRID 1003989 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[O:9][CH3:10].CO[CH2:13][Cl:14].O>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([O:9][CH3:10])=[CH:4][C:5]([CH2:13][Cl:14])=[C:6]([F:8])[CH:7]=1

参加物

6

反応物 3

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 27735802-Chloro-4-fluoroanisole

生成物 1

HCID 184083444-Chloro-2-fluoro-5-methoxybenzyl chloride収率 68%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 24193Titanium Tetrachloride溶媒

実験手順

17.6 g (0.11 mol) of 2-chloro-4-fluoroanisole was dissolved in a dichloromethane solution of 1N titanium tetrachloride, and 88.3 g (1.10 mol) of methoxymethyl chloride was dropwise added thereto at room temperature, followed by stirring at room temperature for 5 hours. after completion of the reaction, the reaction solution was poured into water, followed by stirring at room temperature for 2 hours, and then the aqueous phase was removed. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off. Then, the obtained residue was purified by silica gel column chromatography to obtain 15.5 g (yield: 68%) of the desired product.

後処理

  1. additionwas dropwise added
  2. customat room temperature
  3. customafter completion of the reaction
  4. stirringby stirring at room temperature for 2 hours
  5. customthe aqueous phase was removed
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. customThen, the obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f6c72ed51d9745e391b1b72d0d459a90
出典データセット
uspto-grants-2000_04
特許番号
US06048823

反応ノート

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