Hydrochloric Acid → HCID 17858921, compound

Acetic acid (7 ml) and concentrated hydrochloric acid (7 ml) were added to di-tert-butyl 3-fluoro-5-methoxy-4-nitrophenylmalonate (4.88 g, 12.7 mmol). The mixture was heated under reflux for 15 hours under stirring. After cooling, the reaction mixture was distilled under reduced pressure to remove the solvent. To the residue were added 1N NaOH (200 ml) and ether (200 ml) to separate it into layers. The water layer thus obtained was acidified with 1N HCl, followed by extraction with ether (200 ml). The extract was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, whereby the title compound (2.83 g, 97%) was obtained as a pale brown solid.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 15 hours
3. temperatureAfter cooling
4. distillationthe reaction mixture was distilled under reduced pressure
5. customto remove the solvent
6. additionTo the residue were added 1N NaOH (200 ml) and ether (200 ml)
7. customto separate it into layers
8. customThe water layer thus obtained
9. extractionfollowed by extraction with ether (200 ml)
10. dry with materialThe extract was dried over anhydrous magnesium sulfate
11. distillationdistilled under reduced pressure
12. customto remove the solvent, whereby the title compound (2.83 g, 97%)
13. customwas obtained as a pale brown solid

ORD record

ord-61233eb738b74fcd8123881b35197473

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07157487B2