Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68720375 | HCID 68720375 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 59699472 | HCID 59699472 | 96.8% |
Reaction Steps
A solution of 6N HCl (30 ml, 5.5 eq) was added to a solution of 16 (12.0 g) in 200 ml of MeOH at room temperature, and the reaction mixture was warmed up to 40° C. overnight. Methanol was removed in vacuo. The reaction mixture was washed with diethyl ether (50 ml×2). The aqueous solution was neutralized with 2N NaOH and extracted with ethyl acetate (100 ml×3). The organic layer was washed with brine, dried over sodium sulfate, and concentrated to provide the pure desired product (7.6 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07713950B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-e56939a9fa444f6980f01f69f06f2b94 |
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| Source note | uspto-grants-2010_05 |
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