Hydrochloric Acid → 1-(4-Chlorophenyl)-3-(dimethylamino)propan-1-one

HRID 399887

反応式

HRID 399887 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:15])[CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:5][CH:4]=1.CC(C1C=CC(Cl)=CC=1)=O.Cl.CNC.C=O.Cl>C(O)C.CC(C)=O>[Cl:2][C:3]1[CH:4]=[CH:5][C:6]([C:9](=[O:15])[CH2:10][CH2:11][N:12]([CH3:14])[CH3:13])=[CH:7][CH:8]=1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 7467P-ChloroacetophenoneHCID 10473Dimethylamine, hydrochlorideHCID 2003701-Propanone, 1-(4-chlorophenyl)-3-(dimethylamino)-, hydrochloride (1:1)

生成物 1

HCID 2003711-(4-Chlorophenyl)-3-(dimethylamino)propan-1-one

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒

実験手順

4'-Chloro-3-dimethylaminopropiophenone is prepared by treating 4'-chloro-3-dimethylaminopropiophenone hydrochloride with aqueous base to remove the HCl. The free amine is extracted into diethyl ether and recovered by evaporation of the solvent. The hydrochloride salt is prepared by the method of Maxwell in Org. Synth. Coll. Vol. III, 305-306. Thus, a mixture of 4-chloroacetophenone, dimethylamine hydrochloride, and paraformaldehyde is refluxed for 2-4 hours in 95% ethanol with a small amount of added hydrochloric acid. The solid product is obtained after adding acetone and cooling overnight.

後処理

  1. customto remove the HCl
  2. extractionThe free amine is extracted into diethyl ether
  3. customrecovered by evaporation of the solvent
  4. customThe solid product is obtained
  5. temperaturecooling overnight

出典と根拠

ORDレコード
ord-3c30c644c8ca46be9c860204a7b6da4b
出典データセット
uspto-grants-1998_10
特許番号
US05824744

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