Hydrochloric Acid → 3-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochloride

HRID 236558

반응식

HRID 236558 반응식
[C:1]([C:4]1[S:5][C:6]([CH3:9])=[CH:7][CH:8]=1)(=[O:3])[CH3:2].[ClH:10].[CH3:11][NH:12][CH3:13].[CH2:14]=O.Cl>C(O)C>[ClH:10].[CH3:11][N:12]([CH3:14])[CH2:13][CH2:2][C:1]([C:4]1[S:5][C:6]([CH3:9])=[CH:7][CH:8]=1)=[O:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 836552-Acetyl-5-methylthiophene

생성물 1

HCID 126434363-Dimethylamino-1-(5-methyl-2-thienyl)-propan-1-one hydrochloride수율 65.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Under a nitrogen atmosphere, a stirred solution of 10.0 grams (0.071 mole) of 2-acetyl-5-methylthiophene, 7.0 grams (0.086 mole) of dimethylamine hydrochloride, 2.5 grams of paraformaldehyde and 0.4 ml of concentrated hydrochloric acid in 10 ml of ethanol was heated under reflux for 16 hours. The reaction mixture was concentrated under reduced pressure to a residual solid. The solid was recrystallized from methanol-diethyl ether to give 10.9 grams of 3-dimethylamino-1-(5-methyl-2-thienyl)propan-1-one hydrochloride; m.p. 145°-147° C.

후처리

  1. temperatureunder reflux for 16 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure to a residual solid
  3. customThe solid was recrystallized from methanol-diethyl ether

출처 및 근거

ORD 기록
ord-7533c9036b464e4a94d876df66df5f98
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645777

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