Hydrochloric Acid → HCID 59483836, Verbindung

HRID 1808378Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1808378
Cl.[N:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:37][CH2:36][C:11]3([CH2:16][CH2:15][N:14]([C:17]([C:19]4[CH:28]=[C:27]5[C:22]([CH2:23][CH2:24][N:25](C(OC(C)(C)C)=O)[CH2:26]5)=[CH:21][CH:20]=4)=[O:18])[CH2:13][CH2:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1>CO>[N:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:37][CH2:36][C:11]3([CH2:12][CH2:13][N:14]([C:17]([C:19]4[CH:28]=[C:27]5[C:22]([CH2:23][CH2:24][NH:25][CH2:26]5)=[CH:21][CH:20]=4)=[O:18])[CH2:15][CH2:16]3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 59483838HCID 59483838, Verbindung

Produkt 1

HCID 59483836HCID 59483836, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

1.25 M hydrogen chloride in methanol (15.5 ml, 19.36 mmol) was added at RT to a solution of tert-butyl 7-(9-(pyridin-4-yl)-3,9-diazaspiro[5.5]undecane-3-carbonyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (1.9 g, 3.87 mmol) in methanol (4 ml), and the reaction mixture was refluxed for 1.5 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. The mixture was then cooled for 30 min in an ice bath, and the resulting solid was filtered out, washed with diethyl ether and dried in vacuo. Yield: 1.56 g (94%).

Aufarbeitung

  1. temperaturethe reaction mixture was refluxed for 1.5 h
  2. customThe solvent was removed in vacuo
  3. additionwas added
  4. temperatureThe mixture was then cooled for 30 min in an ice bath
  5. filtrationthe resulting solid was filtered out
  6. washwashed with diethyl ether
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-16cb9eb322f44de5b83f7353ec04cb6d
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08357717B2

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