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

HRID 728053

反応式

HRID 728053 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21584188Chloroform methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-34a3d8d523ea4bd2a7229b76f02fe631
出典データセット
uspto-grants-1991_09
特許番号
US05047431

関連ノート

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