Hydrochloric Acid → 2-(Pyridin-4-yl)-2,9-diazaspiro[5.5]undecane dihydrochloride

HRID 1253676노트

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HRID 1253676 반응식
[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH2:11][C:10]3([CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]3)[CH2:9]2)=[CH:4][CH:3]=1>CO>[ClH:1].[ClH:1].[N:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][CH2:11][C:10]3([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[CH2:9]2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66700745tert-Butyl 2-(pyridin-4-yl)-2,9-diazaspiro[5.5]undecane-9-carboxylate

생성물 1

HCID 667010972-(Pyridin-4-yl)-2,9-diazaspiro[5.5]undecane dihydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

Hydrogen chloride in methanol (1.25 mol/l, 15.9 ml) was added to tert-butyl 2-(pyridin-4-yl)-2,9-diazaspiro[5.5]undecane-9-carboxylate (0.66 g, 1.991 mmol) and the mixture was refluxed for 2 h. The solvent was removed in vacuo, the residue was taken up in ethanol (5 ml) and the mixture was cooled. Acetone (20 ml) was added and the mixture was stirred at 0° C. for 30 min. Diethyl ether (50 ml) was added and the precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo. Yield: 0.42 g (69%)

후처리

  1. temperaturethe mixture was refluxed for 2 h
  2. customThe solvent was removed in vacuo
  3. temperaturethe mixture was cooled
  4. additionAcetone (20 ml) was added
  5. additionDiethyl ether (50 ml) was added
  6. filtrationthe precipitate was filtered out with suction
  7. washwashed with diethyl ether
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-964957be90e743c0ab38c79e05c8a8ef
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455475B2

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