Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 59180392 | HCID 59180392 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 25183517 | HCID 25183517 | 93.3% |
Reaction Steps
To a solution of 71 (1.75 g; 4.5 mmol) in tetrahydrofuran (25 mL) was added aqueous sodium hydroxide (20 mL; 6M) and then heated at 70° C. for 24 hours. The reaction mixture was allowed to cool to room temperature and then acidified to pH 2 with concentrated hydrochloric acid. The organic solvent was removed under reduced pressure and the resulting aqueous solution was extracted with chloroform (3×20 mL). The organic extracts were combined and successively washed with water and aqueous saturated sodium chloride, dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to yield the title compound as an off-white solid (1.57 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08178699B2 |
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| Source dataset | uspto-grants-2012_05 |
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| ORD ID | ord-626c9fac4ebe4aad841f444a1fa29fa4 |
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| Source note | uspto-grants-2012_05 |
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