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

HRID 1379173

반응식

HRID 1379173 반응식
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

참가 물질

8

반응물 5

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-56f9b76dbf344b45980844846a6922d9
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05670564

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