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Hydrochloric Acid → 1-((1S,4S)-2,5-diazabicyclo(2.2.1)heptan-2-yl)ethan-1-one hydrochloride

HRID 1841976
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HRID 1841976 반응식
C([O:5][C:6]([N:8]1[CH2:13][C@@H:12]2[CH2:14][C@H:9]1[CH2:10][NH:11]2)=O)(C)(C)C.[C:15](OC(=O)C)(=O)C.[ClH:22].O1CCOCC1>C(Cl)Cl>[ClH:22].[C@H:9]12[CH2:14][C@H:12]([NH:11][CH2:10]1)[CH2:13][N:8]2[C:6](=[O:5])[CH3:15]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 312751,4-DioxaneHCID 11521263(1S,4S)-2-Boc-2,5-diazabicyclo[2.2.1]heptane

생성물 1

HCID 574640501-((1S,4S)-2,5-diazabicyclo(2.2.1)heptan-2-yl)ethan-1-one hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

To a solution of (1S,4S)-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester (1.00 g, 5.04 mmol) in DCM (15 mL) is added acetic anhydride (0.52 mL, 5.55 mmol) and the reaction stirred at about 25° C. for 72 hours. The reaction is concentrated, and the residue dissolved in DCM (15 mL) and treated with 4M HCl in 1,4-dioxane (5.04 mL, 20.2 mmol). The reaction is stirred overnight, and the solid filtered to afford the title compound (O).

후처리

  1. concentrationThe reaction is concentrated
  2. dissolutionthe residue dissolved in DCM (15 mL)
  3. stirringThe reaction is stirred overnight
  4. filtrationthe solid filtered

출처 및 근거

ORD 기록
ord-f16f360f2a384a0ca84e5f47d0417ac9
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946203B2

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