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

HRID 1253676ノート

反応式

HRID 1253676 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-964957be90e743c0ab38c79e05c8a8ef
出典データセット
uspto-grants-2013_06
特許番号
US08455475B2

反応ノート

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