Phosphorus oxychloride → 4-Chloro-5-iodo-alpha,alpha,alpha-trifluoro-2-picoline
Reaktionsgleichung
[I:1][C:2]1[C:3](O)=[CH:4][C:5]([C:8]([F:11])([F:10])[F:9])=[N:6][CH:7]=1.O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:3]1[C:2]([I:1])=[CH:7][N:6]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:4]=1Komponenten
3
Versuchsvorschrift
A solution of 5-iodo-2-(trifluoromethyl)pyridin-4-ol (4.8 g, 16.6 mmol) in POCl3 (30 mL) was heated to 100° C. for 30 minutes. The resulting solution was concentrated under vacuum and the residue was neutralized by the addition of ice and aqueous potassium carbonate. The solution was extracted with ethyl acetate, dried (Na2SO4), filtered and concentrated under vacuum to give 4-chloro-5-iodo-2-(trifluoromethyl)pyridine. Retention time (min)=2.594, method [1], MS (ESI) 307.9 (M+H).
Aufarbeitung
- concentrationThe resulting solution was concentrated under vacuum
- additionthe residue was neutralized by the addition of ice and aqueous potassium carbonate
- extractionThe solution was extracted with ethyl acetate
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-d3df14058b9644da868c362dc32a2b26
- Quelldatensatz
- uspto-grants-2013_05
- Patentnummer
- US08450363B2
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