Reaktion #1847363
ord-7877366897604b82bf401ee7cccf116e
Reaktionsgleichung
Edukte
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1workup.STIRRINGThe mixture was stirred at 80° C. for 3 h
- 2Extraktionthe whole was extracted with methylene chloride
- 3TrocknenThe organic phase was dried over magnesium sulfate
- 4Einengenconcentrated under reduced pressure
- 5Sonstigethe residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90)
- 6SonstigeThe following was obtained
Vorschrift
7.5 mg of lithium aluminum hydride were initially introduced into 1.5 ml of tetrahydrofuran and the mixture was stirred for 10 min. 6 mg of methyl 5-phenyl-1H-pyrazolo[4,3-c]isoquinoline-3-carboxylate (61) in 1.5 ml of tetrahydrofuran were then added dropwise. The mixture was stirred at 80° C. for 3 h, after which water was added and the whole was extracted with methylene chloride. The organic phase was dried over magnesium sulfate and concentrated under reduced pressure, and the residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90). The following was obtained: 62. C17H13N3O1 (275.31) MS (ESI) 276 (M+H)