2-Chloropropionyl chloride → 2-(1-Chloroethyl)-8-fluoro-4H-3,1-benzoxazin-4-one
Reaktionsgleichung
[NH2:1][C:2]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Cl:12][CH:13]([CH3:17])[C:14](Cl)=O>>[Cl:12][CH:13]([C:17]1[O:5][C:4](=[O:6])[C:3]2[CH:7]=[CH:8][CH:9]=[C:10]([F:11])[C:2]=2[N:1]=1)[CH3:14]Komponenten
3
Versuchsvorschrift
A mixture of 9.3 g of 2-amino-3-fluoro-benzoic acid and 18,6 ml of α-chloropropionyl chloride was refluxed for 3 hours and excess acid chloride was distilled off. The residue was concentrated under reduced pressure at 70° C. for 2 hours to obtain 2-(1-chloroethyl)-8-fluoro-4H-3,1-benzoxazine-4-one which was used as is for the next step.
Aufarbeitung
- temperaturewas refluxed for 3 hours
- distillationexcess acid chloride was distilled off
- concentrationThe residue was concentrated under reduced pressure at 70° C. for 2 hours
Quellen und Nachweise
- ORD-Eintrag
- ord-56f74fbd68384ec0ab21d683e34ef61f
- Quelldatensatz
- uspto-grants-1984_12
- Patentnummer
- US04486438
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