Hydrochloric Acid → HCID 66701057, Verbindung

HRID 1808353Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1808353
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][C:12]2([CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=3)[CH2:16][CH2:15]2)[CH2:11][CH2:10]1)=O)(C)(C)C>CO>[ClH:1].[ClH:1].[N:23]1[CH:22]=[CH:21][C:20]([N:17]2[CH2:18][CH2:19][C:12]3([CH2:13][CH2:14][NH:9][CH2:10][CH2:11]3)[CH2:15][CH2:16]2)=[CH:25][CH:24]=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, and the residue was taken up in ethanol (3 ml) and cooled. Acetone (80 ml) was added and stirring was carried out for 30 min. in an ice bath. The precipitate was filtered out with suction, washed with diethyl ether and dried in vacuo. Yield: 0.4 g (83%) Alternatively, the deprotection can also be carried out under the action of TFA in DCM in order to obtain the amine (F-09) in the form of the free base.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 1 h
  2. customThe solvent was removed in vacuo
  3. temperaturecooled
  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-2837bc3976194ea58b40e907ea7e24aa
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08357717B2

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