Hydrochloric Acid → HCID 66701057, Verbindung

HRID 1643435Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1643435
[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N: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:4][CH:3]=1>CO>[ClH:1].[ClH:1].[N:2]1[CH:3]=[CH:4][C:5]([N: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:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59486425tert-Butyl 9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carboxylate

Produkt 1

HCID 66701057HCID 66701057, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Hydrogen chloride in methanol (1.25 mol/l, 6.3 ml) was added to tert-butyl 9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carboxylate (0.52 g, 1.569 mmol) and the mixture was refluxed for 1 h. The solvent was removed in vacuo, the residue taken up in ethanol (3 ml) and the mixture cooled. Acetone (80 ml) was added and the mixture was stirred in an ice bath for 30 min. The precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. temperaturethe mixture cooled
  4. additionAcetone (80 ml) was added
  5. filtrationThe precipitate was filtered out with suction
  6. washwashed with diethyl ether
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8e634edeb8a440f895568ee0659e5ba6
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08119805B2

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