Hydrogen iodide → HCID 15096982, compound

Temperature

0 °C

30.6 Parts of cyclopropyl (4-fluoro-2-hydroxyphenyl)-methanone were added portionwise to 450 parts of hydroiodic acid solution 50%. The whole was heated to reflux and stirring was continued for 1.50 hours at reflux temperature. The reaction mixture was cooled to 0° C. The precipitated product was filtered off and dissolved in 300 parts of trichloromethane. The solution was dried, filtered and evaporated. The residue was dissolved in 210 parts of petroleumether while heating. The solution was treated twice with activated charcoal and the latter was filtered off each time. The filtrate was evaporated and the residue was suspended in 35 parts of petroleumether. After cooling to 0° C., the product was filtered off and dried, yielding 36.4 parts (70%) of 1-(4-fluoro-2-hydroxyphenyl)-4-iodo-1-butanone; mp. 41.4° C. (intermediate 89).

1. temperatureThe whole was heated
2. temperatureto reflux
3. temperatureat reflux temperature
4. filtrationThe precipitated product was filtered off
5. dissolutiondissolved in 300 parts of trichloromethane
6. customThe solution was dried
7. filtrationfiltered
8. customevaporated
9. dissolutionThe residue was dissolved in 210 parts of petroleumether
10. temperaturewhile heating
11. additionThe solution was treated twice with activated charcoal
12. filtrationthe latter was filtered off each time
13. customThe filtrate was evaporated
14. temperatureAfter cooling to 0° C.
15. filtrationthe product was filtered off
16. customdried

ORD record

ord-92a238d6f87b4311a9adb1c31e987863

Source dataset

uspto-grants-1992_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05137896