Methanol → HCID 10866482, compound

To a solution of the product from Example 94A (5.92 g, 39.2 mmol) in 100 mL of THF was added MeOH (1.26 g, 39.2 mmol). The mixture was heated at reflux for 2 hours then allowed to cool to ambient temperature. The solvent was removed under reduced pressure and the crude product was dissolved in 100 mL of EtOAc/hexanes (1:1). The mixture was filtered through a ½″ silica gel frit and the frit was washed with an additional 50 mL of EtOAc/hexanes (1:1). The solvent was removed in vacuo to provide a pale yellow oil which solidified on standing. The product (4.56 g, 80% crude yield) was used without further purification.

1. temperatureThe mixture was heated
2. temperatureat reflux for 2 hours
3. customThe solvent was removed under reduced pressure
4. dissolutionthe crude product was dissolved in 100 mL of EtOAc/hexanes (1:1)
5. filtrationThe mixture was filtered through a ½″ silica gel frit
6. washthe frit was washed with an additional 50 mL of EtOAc/hexanes (1:1)
7. customThe solvent was removed in vacuo
8. customto provide a pale yellow oil which
9. customThe product (4.56 g, 80% crude yield) was used without further purification

ORD record

ord-543dde20fa554db8b22031c8411e9a05

Source dataset

uspto-grants-2002_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06495576B2