Hydrochloric Acid → 1-(5-Chloro-2,4-dimethoxyphenyl)ethan-1-one

HRID 2257123노트

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HRID 2257123 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[O:10][CH3:11].[C:12](Cl)(=[O:14])[CH3:13].Cl>C(Cl)(Cl)(Cl)Cl.Cl[Ti](Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([O:10][CH3:11])=[CH:4][C:5]([O:8][CH3:9])=[C:6]([C:12](=[O:14])[CH3:13])[CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 1389051-Chloro-2,4-dimethoxybenzene

생성물 1

HCID 24325931-(5-Chloro-2,4-dimethoxyphenyl)ethan-1-one수율 48.4%

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 5943Carbon Tetrachloride용매2회

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온도
0 °C

실험 절차

A mixture of 2 g of 1-chloro-2,4-dimethoxybenzene and 0.9 g of acetyl chloride in 20 ml of CCl4 is cooled to 0° C., and a solution of 1.3 ml of TiCl4 in 7 ml of CCl4 is added dropwise. The reaction mixture is left stirring for 2 hours while the temperature is allowed to rise to r.t. It is poured into a mixture of concentrated HCl and ice, the resulting mixture is extracted with DCM, the organic phase is dried over magnesium sulphate and the solvents are evaporated off under vacuum. The residue is chromatographed on silica H, eluting with a DCM/heptane (70:30; v/v) mixture. 1.19 g of the expected product, m.p.=138° C., are obtained.

후처리

  1. waitThe reaction mixture is left
  2. customto rise to r.t
  3. extractionthe resulting mixture is extracted with DCM
  4. dry with materialthe organic phase is dried over magnesium sulphate
  5. customthe solvents are evaporated off under vacuum
  6. customThe residue is chromatographed on silica H
  7. washeluting with a DCM/heptane (70:30; v/v) mixture

출처 및 근거

ORD 기록
ord-7a6ed299f81c4a6fbce5980aab570c5e
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656648

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