HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 87604842, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 87605505 | HCID 87605505 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 87604842 | HCID 87604842 | — |
Reaction Steps
A mixture of Example 470F (75 mg, 0.2 mmol), lithium hydroxide (70 mg, 2.0 mmol), dioxane (1.5 mL), and water (0.75 mL) was sealed in a vial and microwaved at 160° C. for 15 minutes. Purification by preparative HPLC on a Waters Symmetry C8 column (25 mm×100 mm, 7 μm particle size) using a gradient of 10% to 100% acetonitrile/10 mmol aqueous ammonium acetate over 8 minutes (10 minute run time) at a flow rate of 40 mL/min provided the desired compound. MS (ESI(+)) m/e 432, 434 (M+H)+; (ESI(−)) m/e 430, 432 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.68 (m, 1H), 7.57 (m, 1H), 7.28 (m, 3H), 3.65 (s, 3H), 2.49 (m, 4H), 1.09 (t, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07491718B2 |
| Source dataset | uspto-grants-2009_02 |
| ORD ID | ord-da0347e914624c3b92fb58f1b3f80508 |
| Source note | uspto-grants-2009_02 |