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Chloride → (R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride

HRID 861898
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HRID 861898 반응식
[Cl-:1].[C:2]([CH:5]([CH:7]([C:9](O)=O)O)O)(O)=O.[NH:12]1[CH2:17][CH2:16][CH2:15][C@@H:14]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:13]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[CH3:31][C:32](=O)[CH2:33][CH3:34]>ClCCl>[ClH:1].[CH2:21]([O:20][C:18]([C@@H:14]1[CH2:15][CH2:16][CH2:17][N:12]([CH2:18][CH2:14][CH2:13][N:12]2[C:33]3[CH:34]=[CH:2][CH:5]=[CH:7][C:32]=3[C:31]3[CH:15]=[CH:16][CH:17]=[CH:9][C:7]=3[C:5]3[CH:31]=[CH:32][CH:33]=[CH:34][C:2]2=3)[CH2:13]1)=[O:19])[CH3:22]
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참가 물질

7

반응물 5

HCID 312ChlorideHCID 4875Potassium IodideHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 2733695(R)-(-)-Ethyl Nipecotate Tartrate

생성물 1

HCID 70197521(R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride수율 41%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of the above chloride (0.21 g, 0.66 mmol), ethyl (R)-3-piperidinecarboxylate tartrate (0.30 g, 1.0 mmol), potassium carbonate (0.18 g, 2.0 mmol), potassium iodide (0.10 g, 0.60 mmol) and 2-butanone (10 ml) was heated at reflux temperature for 40 hours. After cooling to room temperature, dichloromethane (50 ml) was added and the mixture was filtered. The filtrate was washed with 1N hydrochloric acid (20 ml), water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml), dried over sodium sulfate and evaporated in vacuo. The remainder was dissolved in diethyl ether (20 ml) and a 2.6M solution of hydrogen chloride in diethyl ether (0.5 ml) was added. The formed precipitate was collected by filtration, washed with ether and dried, affording 0.13 g (41%) of (R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride as a solid.

후처리

  1. temperaturewas heated
  2. temperatureat reflux temperature for 40 hours
  3. filtrationthe mixture was filtered
  4. washThe filtrate was washed with 1N hydrochloric acid (20 ml), water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml)
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. dissolutionThe remainder was dissolved in diethyl ether (20 ml)
  8. additiona 2.6M solution of hydrogen chloride in diethyl ether (0.5 ml) was added
  9. filtrationThe formed precipitate was collected by filtration
  10. washwashed with ether
  11. customdried

출처 및 근거

ORD 기록
ord-885e18a385c04b4aa8a8944b0ead5801
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05716949

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