Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 67256120 | HCID 67256120 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67255853 | HCID 67255853 | — |
Reaction Steps
To a mixed solution of the compound prepared in Example 45 (413 mg) in acetic acid (7.6 mL)-N,N-dimethylformamide (7.0 mL) was added ammonium acetate (1.18 g) and the mixture was stirred at 100° C. for an hour. The reaction mixture was poured into 5N aqueous solution of sodium hydroxide and the mixture was extracted with ethyl acetate. After having made the water layer acidity with 2N hydrochloric acid, the mixture was extracted with ethyl acetate. The organic layer was put together, washed with brine, dried and concentrated. The obtained residue was purified by preparative medium pressure liquid chromatography W-prep 2XY (column: main column L, inject column M; automatic condition setting: hexane:ethyl acetate=1:1, Rf=0.30, preparative isolation mode GR) to give the title compound having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07968572B2 |
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| Source dataset | uspto-grants-2011_06 |
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| ORD ID | ord-1c2d291006c1422a8f5d74f5ec4e4647 |
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| Source note | uspto-grants-2011_06 |
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