Hydrochloric Acid → HCID 22163783, 화합물

HRID 1087821

반응식

HRID 1087821 반응식
[C:1](N1C=CN=C1)(N1C=CN=C1)=[O:2].[NH2:13][CH2:14][CH2:15][N:16]1[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.[C:23]1([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[ClH:35]>O1CCCC1>[ClH:35].[N:16]1([CH2:15][CH2:14][NH:13][C:1]([N:32]2[CH2:33][CH2:34][N:29]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:30][CH2:31]2)=[O:2])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 70961-PhenylpiperazineHCID 40002Hexahydro-1H-azepine-1-ethanamineHCID 682631,1'-Carbonyldiimidazole

생성물 1

HCID 22163783HCID 22163783, 화합물수율 53%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a solution of 5.0 g (0.03 mole) of 1,1'-carbonyldiimidazole in 75 ml of tetrahydrofuran (THF) was added a solution of 4.0 g (0.028 mole) of N-(2-aminoethyl)homopiperidine in 75 ml of THF, and the reaction mixture was stirred at ambient temperature for 1.5 hr. A solution of 5.0 g (0.03 mole) of 1-phenylpiperazine in 50 ml of THF was added, and the reaction mixture was heated at reflux for 20 hr. The solution was concentrated under reduced pressure, and the residue was dissolved in 150 ml of benzene. The solution was washed thrice with 50 ml portions of water and once with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give an oil, which was converted to the hydrochloride with ethereal hydrogen chloride. The collected solid was recrystallized from 2-propanol to yield 6.7 g (53%) of title compound as a white solid, m.p. 190°-193° C.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 20 hr
  3. concentrationThe solution was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in 150 ml of benzene
  5. washThe solution was washed thrice with 50 ml portions of water
  6. dry with materialonce with brine, dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto give an oil, which
  9. customThe collected solid was recrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-eaebc368edf44efda0dd3b466f1baedd
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960776

연결된 노트

불러오는 중…