Phosphorus oxychloride → Methyl 1-chloro-4-hydroxyisoquinoline-3-carboxylate
Reaktionsgleichung
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5](=O)[NH:4][C:3]=1[C:13]([O:15][CH3:16])=[O:14].P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:2]([OH:1])=[C:3]([C:13]([O:15][CH3:16])=[O:14])[N:4]=1Komponenten
3
Versuchsvorschrift
2.84 g (13 mmol) of methyl 4-hydroxy-1 (2H)-isoquinolone-3-carboxylate (prepared as in M. Suzuki, SYNTHESIS, 461 (1978)) was stirred at 70° C. for 3 h in 25 ml of phosphorus oxychloride. After cooling, the mixture was added to 500 ml of ice water, the precipitate was filtered off with suction next morning and dried at 70° C. under an IR Lamp. 2.96 g of product were obtained; m.p. 168° C.
Aufarbeitung
- temperatureAfter cooling
- filtrationthe precipitate was filtered off with suction next morning
- customdried at 70° C. under an IR Lamp