Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 69307065 | HCID 69307065 | — |
| Solvent | Methanol tetrahydrofuran water | HCID 21892291 | — |
| Product | HCID 69308244 | HCID 69308244 | — |
Reaction Steps
To a THF/MeOH/water solution (ca. 40 mL/40 mL/10 mL) of the intermediate from Step F (8.53 g, 17.84 mmol) was added LiOH (3.66 g, 89.2 mmol). The solution was stirred at 45° C. until no starting material remained by HPLC (ca. 2 hrs). The solution was concentrated to remove the majority of MeOH/THF and then partitioned between aqueous 1N HCl and ethyl acetate. The organic phase was washed with water (2×), brine and dried over Na2SO4. The solution was filtered and concentrated to give the title compound. The crude material was use in the next step without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08318760B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-e8733e65d7a74972b7e8f3e9db8f2b37 |
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| Source note | uspto-grants-2012_11 |
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