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

HRID 992903노트

반응식

HRID 992903 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 184083444-Chloro-2-fluoro-5-methoxybenzyl chloride수율 68%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 24193Titanium Tetrachloride용매

실험 절차

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.

후처리

  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 The organic layer
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. customThen, the obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4e75cf6b6849448486d1734f943a47e4
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472348B1

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