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

HRID 370742

반응식

HRID 370742 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e821cf1d067e446f94e7cc973f1392ee
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528299

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