Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 68864035 | HCID 68864035 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68865836 | HCID 68865836 | — |
Reaction Steps
A solution of Example 463A (1.37 g, 3.36 mmol) in methanol (31 mL) and distilled water (3.5 mL) was treated with lithium hydroxide monohydrate (0.704 g, 16.78 mmol), heated to 60° C. for 30 minutes, cooled to room temperature, treated with 1N HCl, and concentrated. The aqueous layer was extracted with dichloromethane twice and the combined organic fractions were dried (MgSO4), filtered, and concentrated to provide the desired product. MS (ESI(+)) m/e 396 (M+H)+; (ESI(−)) m/e 394 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 8.98 (br s, 1H), 7.89 (d, 1H), 7.33 (d, 1H), 7.12 (s, 2H), 3.77 (s, 3H), 2.67 (br s, 2H), 2.53 (br s, 2H), 1.65 (quint, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07491718B2 |
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| Source dataset | uspto-grants-2009_02 |
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| ORD ID | ord-10b5df9deeb149fca45b0868351c6277 |
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| Source note | uspto-grants-2009_02 |
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