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Hydrogen chloride-ethyl acetate → HCID 86678702, 화합물

HRID 1620509
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HRID 1620509 반응식
[OH:1][CH2:2][CH:3]1[CH2:10][CH:9]2[CH2:11][CH:5]([CH2:6][N:7](C(OC(C)(C)C)=O)[CH2:8]2)[CH2:4]1.[ClH:19].C(OCC)(=O)C>CO>[ClH:19].[CH:9]12[CH2:11][CH:5]([CH2:4][CH:3]([CH2:2][OH:1])[CH2:10]1)[CH2:6][NH:7][CH2:8]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86678701HCID 86678701, 화합물

생성물 1

HCID 86678702HCID 86678702, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 3-tert-butyl 7-hydroxymethyl-3-azabicyclo[3.3.1]nonane-3-carboxylate (7.78 g) in methanol (76 mL) was added 4M hydrogen chloride/ethyl acetate solution (76 mL). The reaction mixture was stirred at room temperature for 4 hr, and the solvent was evaporated under reduced pressure. The residue was dissolved in methanol (50 mL), and Amberlyst A-21 was added. The mixture was stirred at room temperature for 20 min, and the solid was removed by filtration. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethanol/ethyl acetate to give the title compound (5.22 g).

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후처리

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (50 mL)
  3. additionAmberlyst A-21 was added
  4. stirringThe mixture was stirred at room temperature for 20 min
  5. customthe solid was removed by filtration
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was recrystallized from ethanol/ethyl acetate

출처 및 근거

ORD 기록
ord-189db74387ae42bab70b3163274221e0
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772277B2

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