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Hydrochloric Acid → (R)-1-(3-(9H-Tribenz[b,d,f]azepine-9-yl)propyl)-3-piperidinecarboxylic acid, hydrochloride

HRID 861899
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HRID 861899 반응식
[ClH:1].C([O:4][C:5]([C@@H:7]1[CH2:12][CH2:11][CH2:10][N:9]([CH2:13][CH2:14][CH2:15][N:16]2[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[C:20]3[CH:27]=[CH:28][CH:29]=[CH:30][C:19]=3[C:18]3[CH:31]=[CH:32][CH:33]=[CH:34][C:17]2=3)[CH2:8]1)=[O:6])C.Cl>C(O)C.[OH-].[Na+]>[ClH:1].[CH:30]1[C:19]2[C:18]3[CH:31]=[CH:32][CH:33]=[CH:34][C:17]=3[N:16]([CH2:15][CH2:14][CH2:13][N:9]3[CH2:10][CH2:11][CH2:12][C@@H:7]([C:5]([OH:6])=[O:4])[CH2:8]3)[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[C:20]=2[CH:27]=[CH:28][CH:29]=1
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 70197521(R)-1-(3-(9H-tribenz[b,d,f]azepin-9-yl)propyl)-3-piperidine carboxylic acid ethyl ester hydrochloride

생성물 1

HCID 131720461(R)-1-(3-(9H-Tribenz[b,d,f]azepine-9-yl)propyl)-3-piperidinecarboxylic acid, hydrochloride수율 74.2%

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 14798
Sodium Hydroxide
용매

실험 절차

The above ester (0.13 g, 0.27 mmol) was dissolved in ethanol (3 ml) and 2N sodium hydroxide (0.6 ml). The mixture was stirred at room temperature for 1.5 hour, acidified by addition of 1N hydrochloric acid (pH 1) and ethanol was removed in vacuo. The aqueous solution was diluted with water (10 ml), washed with diethyl ether (20 ml) and extracted with dichloromethane (30 ml). The organic extract was dried (MgSO4) and concentrated in vacuo to afford 90 mg (74%) of the title compound as a solid.

후처리

  1. customwas removed in vacuo
  2. additionThe aqueous solution was diluted with water (10 ml)
  3. washwashed with diethyl ether (20 ml)
  4. extractionextracted with dichloromethane (30 ml)
  5. extractionThe organic extract
  6. dry with materialwas dried (MgSO4)
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-77571e7262b9455bb2c38e4b470233f3
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05716949

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