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

HRID 2257123ノート

反応式

HRID 2257123 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 5943Carbon Tetrachloride溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a6ed299f81c4a6fbce5980aab570c5e
出典データセット
uspto-grants-1997_08
特許番号
US05656648

反応ノート

読み込み中…