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Hydrochloric Acid → 1-((3R,4R)-3-amino-4-methoxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone

HRID 1666677
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HRID 1666677 반응식
[CH3:1][O:2][C@H:3]1[C@H:7]([NH:8]C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH2:6][N:5]([C:28](=[O:41])[CH2:29][C:30]2[CH:35]=[CH:34][C:33]([O:36][C:37]([F:40])([F:39])[F:38])=[CH:32][CH:31]=2)[CH2:4]1.Cl>C(OCC)C>[NH2:8][C@H:7]1[C@H:3]([O:2][CH3:1])[CH2:4][N:5]([C:28](=[O:41])[CH2:29][C:30]2[CH:31]=[CH:32][C:33]([O:36][C:37]([F:38])([F:39])[F:40])=[CH:34][CH:35]=2)[CH2:6]1
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HCID 313Hydrochloric AcidHCID 674430721-((3R,4R)-3-Methoxy-4-(tritylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone

생성물 1

HCID 579701661-((3R,4R)-3-amino-4-methoxypyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone수율 94.8%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

1-((3R,4R)-3-Methoxy-4-(tritylamino)pyrrolidin-1-yl)-2-(4-trifluoromethoxyphenyl)ethanone (0.65 g) was dissolved in diethyl ether (5 mL), followed by addition of 5 M hydrochloric acid (5 mL), and the mixture was stirred at room temperature for 17 h. The layers were separated, and the aqueous layer was washed with diethyl ether, 1 M aqueous sodium hydroxide was added to make it basic, and the mixture was extracted with chloroform. The organic layer was dried with anhydrous magnesium sulfate, the desiccant was removed by filtration, and then the filtrate was concentrated under reduced pressure to obtain the title compound (0.35 g).

후처리

  1. customThe layers were separated
  2. washthe aqueous layer was washed with diethyl ether, 1 M aqueous sodium hydroxide
  3. additionwas added
  4. extractionthe mixture was extracted with chloroform
  5. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  6. customthe desiccant was removed by filtration
  7. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7e5e8d755cf04ed3aa377cd520e071b6
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044068B2

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