Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 58424987 | HCID 58424987 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 58424886 | HCID 58424886 | 88.7% |
Reaction Steps
The compound (440 mg, 1.20 mmol) prepared in step 1 was dissolved in excess trifluoroacetic acid (3 ml), and the resulting mixture was heated at 100° C. for 18 hours in sealed-tube. The mixture was poured into ice water and acidified with 2 N sodium hydroxide aqueous solution. After neutralizing with 2 N hydrochloric acid aqueous solution, the crude solution was extracted with dichloromethane and washed with brine. The organic layer was dried over anhydrous sodium sulfate and concentrated to dryness. The residue was then purified by flash column chromatography (dichloromethane:methanol=10:1) to obtain the title compound (260 mg, yield: 88%, white solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08815891B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-993ca8873a5f44fc8ae52f4a64f252b7 |
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| Source note | uspto-grants-2014_08 |
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