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

HRID 280851

반응식

HRID 280851 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fceeae5d0a084f80983d12bee13e820c
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04591590

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