Hydrochloric Acid → 1-(2,4-Dimethoxy-5-methylphenyl)-2-chloro-1-ethanone

HRID 2257121

反応式

HRID 2257121 の反応式
[Al+3].[Cl-].[Cl-].[Cl-].[CH3:5][O:6][C:7]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:8]=1[CH3:15].[Cl:16][CH2:17][C:18](Cl)=[O:19].Cl>ClCCCl.[Cl-].[Cl-].[Zn+2]>[CH3:14][O:13][C:11]1[CH:12]=[C:7]([O:6][CH3:5])[C:8]([CH3:15])=[CH:9][C:10]=1[C:18](=[O:19])[CH2:17][Cl:16]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6577Chloroacetyl chlorideHCID 96403Benzene, 2,4-dimethoxy-1-methyl-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 190280151-(2,4-Dimethoxy-5-methylphenyl)-2-chloro-1-ethanone

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 111,2-Dichloroethane溶媒3 回

反応条件

温度
0 °C

実験手順

A suspension of 5.24 g of AlCl3 and 0.52 g of ZnCl2 in 40 ml of 1,2-dichloroethane is cooled to 0° C., and a solution of 5.0 g of 2,4-dimethoxytoluene in 20 ml of 1,2-dichloroethane is added dropwise. The mixture is then cooled to -10° C., and a solution of 2.9 ml of chloroacetyl chloride in 1.5 ml of 1,2-dichloroethane is added dropwise while the temperature of the reaction medium is maintained at between -10° C. and -7° C. The mixture is left stirring while the temperature is allowed to rise to r.t., the reaction medium is poured into a mixture of ice and concentrated HCl, the resulting mixture is extracted with DCM, the combined organic phases are washed with water and dried over magnesium sulphate and the solvents are evaporated off under vacuum. The residue is taken up in heptane and the precipitate formed is filtered off. 3.0 g of the expected product, m.p.=166°-167° C., are obtained.

後処理

  1. temperatureThe mixture is then cooled to -10° C.
  2. temperatureis maintained at between -10° C. and -7° C
  3. waitThe mixture is left
  4. customto rise to r.t.
  5. extractionthe resulting mixture is extracted with DCM
  6. washthe combined organic phases are washed with water
  7. dry with materialdried over magnesium sulphate
  8. customthe solvents are evaporated off under vacuum
  9. customthe precipitate formed
  10. filtrationis filtered off

出典と根拠

ORDレコード
ord-e80e0e360fcb46a1a35cd7976d080b65
出典データセット
uspto-grants-1997_08
特許番号
US05656648

関連ノート

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