Hydrogen Bromide → (+/-)-9-Amino-2-pyrimidin-4-yl-6,7,8,9-tetrahydro-5H-1,4a,7-triaza-benzocyclohepten-4-one dihydrobromide
Reaktionsgleichung
C(OC([N:6]1[CH2:12][CH:11]([NH2:13])[C:10]2=[N:14][C:15]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][N:20]=3)=[CH:16][C:17](=[O:18])[N:9]2[CH2:8][CH2:7]1)=O)C.[BrH:25]>C(O)(=O)C>[BrH:25].[BrH:25].[NH2:13][CH:11]1[C:10]2=[N:14][C:15]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][N:20]=3)=[CH:16][C:17](=[O:18])[N:9]2[CH2:8][CH2:7][NH:6][CH2:12]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
To a solution of 9.70 g (23.59 mmol) of (+/−)-9-amino-4-oxo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-4H-1,4a,7-triaza-benzocycloheptene-7-carboxylic acid ethyl ester (step 1.4) dissolved in 118 mL of glacial acetic acid was added 41.38 mL (235.86 mmol) of hydrobromic acid (33 wt % solution in glacial acetic acid). The resulting mixture was stirred at 90° C. for 16 hours, cooled and evaporated to dryness. Toluene was added to the residue and evaporated. Ethanol was added to the residue and evaporated. The crude was triturated with diethyl ether and filtered to afford 12.40 g of the product as a brown powder.
Aufarbeitung
- temperaturecooled
- customevaporated to dryness
- additionToluene was added to the residue
- customevaporated
- additionEthanol was added to the residue
- customevaporated
- customThe crude was triturated with diethyl ether
- filtrationfiltered
Quellen und Nachweise
- ORD-Eintrag
- ord-632c5309b1a741eba52eb6ca86f4ec7d
- Quelldatensatz
- uspto-grants-2013_08
- Patentnummer
- US08507475B2
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