HCID 59006711, compound → HCID 59006697, compound

The title compound of Example 36.1 (18.2 g, 59 mmol) was dissolved in acetic acid (95 mL) in a 500 mL two neck flask. Zinc powder (7.6 g, 116 mmol) was added in one portion. The temperature of the mixture reached 60° C. The reaction was complete after 30 min. The mixture was filtered and pentane (200 mL) and water (200 mL) were added. The phases were separated and the water phase washed once again with pentane. The organic phases were combined and washed with sodium hydrogen carbonate solution until pH was neutral, dried (MgSO4), filtered and concentration on reduced-pressure evaporator to give a yellow oil. Yield 82%, 10.2 g.

1. customreached 60° C
2. filtrationThe mixture was filtered
3. additionpentane (200 mL) and water (200 mL) were added
4. customThe phases were separated
5. washthe water phase washed once again with pentane
6. washwashed with sodium hydrogen carbonate solution until pH
7. dry with materialdried (MgSO4)
8. filtrationfiltered
9. concentrationconcentration
10. customon reduced-pressure evaporator
11. customto give a yellow oil

ORD record

ord-8639de65f37a436f9d9b3ea3f225f8e3

Source dataset

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07678796B2