Hydrochloric Acid → 1-Propanone, 1-(4-methoxy-2,3-dimethylphenyl)-

HRID 370742

反応式

HRID 370742 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[C:11](Cl)(=[O:14])[CH2:12][CH3:13].[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(=S)=S>[CH3:8][C:7]1[C:2]([CH3:1])=[C:3]([O:9][CH3:10])[CH:4]=[CH:5][C:6]=1[C:11](=[O:14])[CH2:12][CH3:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 62324Propionyl chlorideHCID 762692,3-DimethylanisoleHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 133066961-Propanone, 1-(4-methoxy-2,3-dimethylphenyl)-収率 91.7%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

To a stirred solution of 2,3-dimethylanisole (197.0 g) and propionyl chloride (147.0 g) in carbon disulfide (700 ml) is added anhydrous aluminum chloride (232.0 g) at 5°-10° C. over a period of 1.5 hours. Stirring is continued for 2 hours under cooling and additional 3 hours at room temperature. The reaction mixture is poured onto crushed ice--concentrated hydrochloric acid with stirring. The mixture is extracted with chloroform and the chloroform solution is washed successively with water, dilute sodium bicarbonate solution and water and then dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue is distilled at 121°-126° C. (1-2 mmHg) to give the title compound (255.0 g), which is crystallized from n-hexane, m.p. 39°-40° C.

後処理

  1. additionThe reaction mixture is poured
  2. customonto crushed ice
  3. extractionThe mixture is extracted with chloroform
  4. washthe chloroform solution is washed successively with water, dilute sodium bicarbonate solution and water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customAfter removal of the solvent
  7. customby evaporation
  8. distillationthe residue is distilled at 121°-126° C. (1-2 mmHg)

出典と根拠

ORDレコード
ord-e821cf1d067e446f94e7cc973f1392ee
出典データセット
uspto-grants-1985_07
特許番号
US04528299

関連ノート

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