Hydrochloric Acid → 1,2,3,4-Tetrahydro-isoquinoline-7-carboxylic acid (4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-yl)-amide hydrochloride

HRID 1886967Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1886967
C(OC([N:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([C:18](=[O:38])[NH:19][CH:20]3[C:26]4=[N:27][C:28]([C:32]5[CH:37]=[CH:36][N:35]=[CH:34][N:33]=5)=[CH:29][C:30](=[O:31])[N:25]4[CH2:24][CH2:23][O:22][CH2:21]3)=[CH:13][CH:14]=2)[CH2:9]1)=O)(C)(C)C.[ClH:39]>ClCCl>[ClH:39].[O:31]=[C:30]1[N:25]2[C:26]([CH:20]([NH:19][C:18]([C:12]3[CH:11]=[C:10]4[C:15]([CH2:16][CH2:17][NH:8][CH2:9]4)=[CH:14][CH:13]=3)=[O:38])[CH2:21][O:22][CH2:23][CH2:24]2)=[N:27][C:28]([C:32]2[CH:37]=[CH:36][N:35]=[CH:34][N:33]=2)=[CH:29]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 44159737HCID 44159737, Verbindung

Produkt 1

HCID 866498491,2,3,4-Tetrahydro-isoquinoline-7-carboxylic acid (4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-yl)-amide hydrochlorideAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 0.049 g (0.10 mmol) of (+/−)-7-(4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-7-oxa-1,4-a-diaza-benzocyclohepten-9-ylcarbamoyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (example 1) dissolved in 0.5 mL of dichloromethane was added 0.24 mL (0.96 mmol) of hydrochloric acid (4M in dioxane). The resulting mixture was stirred at room temperature for 2.5 hours. The resulting residue was filtered, washed with dichloromethane and isopropylether to afford 0.031 g (70%) of the pure product as a yellow powder.

Aufarbeitung

  1. filtrationThe resulting residue was filtered
  2. washwashed with dichloromethane and isopropylether

Quellen und Nachweise

ORD-Eintrag
ord-54a47bbc66724967a22e644acfdf4d13
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501728B2

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