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

HRID 236558

反応式

HRID 236558 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7533c9036b464e4a94d876df66df5f98
出典データセット
uspto-grants-1987_02
特許番号
US04645777

関連ノート

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