Hydrochloric Acid → (9-(Pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)(4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl)methanone hydrochloride

HRID 1808369Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1808369
[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:36][CH2:35][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[S:27][C:26]5[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22][C:21]=5[CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[ClH:1].[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:36][CH2:35][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[S:27][C:26]5[CH2:25][CH2:24][NH:23][CH2:22][C:21]=5[CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59483855HCID 59483855, Verbindung

Produkt 1

HCID 68507109(9-(Pyridin-4-yl)-3,9-diazaspiro[5.5]undecan-3-yl)(4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl)methanone hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

Hydrogen chloride in methanol (2.3 ml, 2.82 mmol, 1.25 mol/l) was added at room temperature to a solution of tert-butyl 2-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)-6,7-dihydrothieno[3,2-c]pyridine-5(4H)-carboxylate (280 mg, 0.564 mmol) in methanol (2 ml), and the reaction mixture was refluxed for 2 h. The solvent was removed in vacuo, the residue was taken up in a small amount of ethanol (3 ml), and diethyl ether (50 ml) was added thereto. Cooling was then carried out for 30 min. in an ice bath, and the resulting solid was filtered out, washed with diethyl ether and dried in vacuo. Yield: 180 mg (73%)

Aufarbeitung

  1. temperaturethe reaction mixture was refluxed for 2 h
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureCooling
  5. filtrationthe resulting solid was filtered out
  6. washwashed with diethyl ether
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c2f8bdfde81a497fa7a66590f9910aea
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08357717B2

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