Hydrochloric Acid → (+/-)-4-Oxo-2-pyridin-4-yl-9-[(1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester

HRID 1890404Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1890404
[CH2:1]([O:3][C:4]([N:6]1[CH2:12][CH:11]([NH:13][C:14]([C:16]2[CH:25]=[C:24]3[C:19]([CH2:20][CH2:21][N:22](C(OC(C)(C)C)=O)[CH2:23]3)=[CH:18][CH:17]=2)=[O:15])[C:10]2=[N:33][C:34]([C:38]3[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=3)=[CH:35][C:36](=[O:37])[N:9]2[CH2:8][CH2:7]1)=[O:5])[CH3:2].Cl>ClCCl>[CH2:1]([O:3][C:4]([N:6]1[CH2:12][CH:11]([NH:13][C:14]([C:16]2[CH:25]=[C:24]3[C:19]([CH2:20][CH2:21][NH:22][CH2:23]3)=[CH:18][CH:17]=2)=[O:15])[C:10]2=[N:33][C:34]([C:38]3[CH:39]=[CH:40][N:41]=[CH:42][CH:43]=3)=[CH:35][C:36](=[O:37])[N:9]2[CH2:8][CH2:7]1)=[O:5])[CH3:2]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 44159005HCID 44159005, Verbindung

Produkt 1

HCID 44159256(+/-)-4-Oxo-2-pyridin-4-yl-9-[(1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl esterAusbeute 1.186,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 0.0265 g (0. mmol) of (+/−)-9-[(2-tert-butoxycarbonyl-1,2,3,4-tetrahydro-isoquinoline-7-carbonyl)-amino]-4-oxo-2-pyridin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester (example 5) dissolved in 1 mL of dichloromethane was added 1.13 mL (4.50 mmol) of hydrochloric acid (4M in dioxane). The resulting mixture was stirred at room temperature for 16 hours. The resulting residue was filtered, washed with dichloromethane and isopropylether to afford 0.261 g (100%) of the pure product as a white powder.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-2abe86c3552d424dafa1ef63fbac1e65
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08507475B2

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