Iodine → HCID 11845284、化合物

Into a reactor, equipped with a mechanic stirrer and a reflux condenser, 8-fluoro-2H-chromene-5-carboxylic acid amide (120 g;0.609 moles), sodium nitrite (96.6 g; 1.4 moles), iodine (31.2 g; 0.123 moles) and ethyl acetate (720 ml) were charged at room temperature and under inert gas. The mixture was heated under stirring at 40° C., then Oxistrong 15® (173.4 g) was added in 4 hours. At the end of the addition the reaction mixture was kept under stirring for 1 hour, then cooled at 20° C. Water (480 ml) was added and the mixture was kept under stirring for 1 hour. After filtration and wash of the panel with isopropyl acetate pre-cooled at 0° C. (2×120 ml) and then with water (150 ml), the solid was dried in oven under vacuum at 50° C. overnight obtaining 8-fluoro-3-nitro-2H-chromene-5-carboxylic acid amide (112.7 g; titre 91%; 70% yield).

1. customInto a reactor, equipped with a mechanic stirrer and a reflux condenser
2. temperatureThe mixture was heated
3. additionOxistrong 15® (173.4 g) was added in 4 hours
4. additionAt the end of the addition the reaction mixture
5. stirringunder stirring for 1 hour
6. temperaturecooled at 20° C
7. stirringunder stirring for 1 hour
8. filtrationAfter filtration
9. washwash of the panel with isopropyl acetate
10. temperaturepre-cooled at 0° C. (2×120 ml)
11. dry with materialwith water (150 ml), the solid was dried in oven under vacuum at 50° C. overnight

ORDレコード

ord-b2ed860c7bb445bcba1e92a082950aaf

出典データセット

uspto-grants-2007_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07265251B2