Hydrochloric Acid → 1-(3-Benzoylaminopropyl)-4-benzhydrylpiperazine dihydrochloride

HRID 280851

反応式

HRID 280851 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][N:8]([CH:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:7][CH2:6]1.[C:24]([Cl:32])(=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.[ClH:33]>N1C=CC=CC=1.C(Cl)(Cl)Cl>[ClH:32].[ClH:33].[C:24]([NH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:6][CH2:7][N:8]([CH:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH2:9][CH2:10]1)(=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 137677783-(4-Benzhydryl-1-piperazinyl)-1-propanamine

生成物 1

HCID 233201841-(3-Benzoylaminopropyl)-4-benzhydrylpiperazine dihydrochloride

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 1-(3-aminopropyl)-4-benzhydrylpiperazine (1.2 g) in a mixture of pyridine (2 ml) and chloroform (15 ml) was dropwise added a solution of benzoyl chloride (0.55 ml) in chloroform (3 ml) at ambient temperature with stirring, which was continued for 1.5 hours. The reaction mixture was washed successively with aqueous sodium bicarbonate and water. The chloroform layer was separated, dried and evaporated in vacuo to give an oil. According to a conventional manner, the oil was converted to hydrochloric acid salt, which was recrystallized from a mixture of methanol and diethyl ether to afford 1-(3-benzoylaminopropyl)-4-benzhydrylpiperazine dihydrochloride (1.0 g) as white crystals. mp: 235°-237° C.

後処理

  1. washThe reaction mixture was washed successively with aqueous sodium bicarbonate and water
  2. customThe chloroform layer was separated
  3. customdried
  4. customevaporated in vacuo
  5. customto give an oil
  6. customwas recrystallized from a mixture of methanol and diethyl ether

出典と根拠

ORDレコード
ord-fceeae5d0a084f80983d12bee13e820c
出典データセット
uspto-grants-1986_05
特許番号
US04591590

関連ノート

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