Hydrochloric Acid → 1-(4-Methoxyphenyl)-2-phenylethan-1-one

HRID 728053

반응식

HRID 728053 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:9]1([CH2:15][C:16](Cl)=[O:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(Cl)(Cl)Cl.CO.C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:16](=[O:17])[CH2:15][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7519AnisoleHCID 7679Phenylacetyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 2310931-(4-Methoxyphenyl)-2-phenylethan-1-one

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 21584188Chloroform methanol용매

실험 절차

To 10.8 g (0.10 mole) methoxybenzene and 13.9 g. (0.09 mole) phenylacetyl chloride in 1.0 1. methylene chloride there are added, by small amounts, 13.3 g. (0.10 mole) aluminium chloride at room temperature and with strong agitation. The reaction mixture is agitated for a further 2 hours and then is poured onto ice and 50 ml. hydrochloric acid are added. After separation of the organic phase, the aqueous solution is shaken out twice with 500 ml. methylene chloride each time, the combined organic phases are washed with water and the solvent is removed in vacuo. The smeary residue is freed of the volatile components by steam distillation and the remaining solid is crystallized from ethanol after filtration and washing with water. Obtained are colorless crystals having a melting point of 75° C.; Rf 0.7 [CHCl3 /CH3OH (9/1)]; yield: 18.3 g. (90%).

후처리

  1. customat room temperature
  2. additionis poured onto ice and 50 ml
  3. customAfter separation of the organic phase
  4. stirringthe aqueous solution is shaken out twice with 500 ml
  5. washmethylene chloride each time, the combined organic phases are washed with water
  6. customthe solvent is removed in vacuo
  7. distillationThe smeary residue is freed of the volatile components by steam distillation
  8. customthe remaining solid is crystallized from ethanol
  9. filtrationafter filtration
  10. washwashing with water
  11. customObtained

출처 및 근거

ORD 기록
ord-34a3d8d523ea4bd2a7229b76f02fe631
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05047431

연결된 노트

불러오는 중…