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Hydrochloric Acid → 9-Pyridin-4-yloxy-3-azaspiro[5.5]undecane dihydrochloride

HRID 1517372
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HRID 1517372 반응식
[N:1]1[CH:6]=[CH:5][C:4]([O:7][CH:8]2[CH2:25][CH2:24][C:11]3([CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:3][CH:2]=1.[ClH:26]>CO>[ClH:26].[ClH:26].[N:1]1[CH:2]=[CH:3][C:4]([O:7][CH:8]2[CH2:25][CH2:24][C:11]3([CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:5][CH:6]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66701182tert-Butyl 9-(pyridin-4-yloxy)-3-azaspiro[5.5]undecane-3-carboxylate

생성물 1

HCID 667544709-Pyridin-4-yloxy-3-azaspiro[5.5]undecane dihydrochloride

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
0 °C

실험 절차

tert-Butyl 9-(pyridin-4-yloxy)-3-azaspiro[5.5]undecane-3-carboxylate (1 g, 2.886 mmol) was dissolved in methanol (2 ml), hydrogen chloride in methanol (1.25 mol/l, 11.5 ml) was added and the mixture was refluxed for 30 min. The solvent was removed in vacuo and the residue was dissolved in a small amount of ethanol. Acetone (approx. 25 ml) was then added, the mixture was stirred at 0° C. for 30 min and the solid formed was finally filtered off with suction. Yield: 0.96 g (>99%)

후처리

  1. temperaturethe mixture was refluxed for 30 min
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in a small amount of ethanol
  4. additionAcetone (approx. 25 ml) was then added
  5. customthe solid formed
  6. filtrationwas finally filtered off with suction

출처 및 근거

ORD 기록
ord-24207cb44b1f45c084fa3b6edf4ab9fc
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232288B2

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