HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 71523551, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 131731659 | HCID 131731659 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 71523551 | HCID 71523551 | 4.71% |
Reaction Steps
A mixture of Example 220B (200 mg, 0.609 mmol) in MeOH (25 mL) was added to Ra—Ni 2800, (water slurry, 500 mg, 9.93 mmol) in a 50 mL pressure bottle and stirred for 16 hours at 30 psi at room temperature, and filtered through a nylon membrane. The filtrate was concentrated and purified using a Waters C8 OBD SunFire 30 mm×75 mm column eluted with acetonitrile/0.1% TFA to afford Example 220C in 4.71% yield. MS (ESI+) M/Z 314 (M+H)+. 1H NMR (300 MHz, DMSO-d6) δ ppm 7.58 (d, J=8.3 Hz, 1H), 7.52 (d, J=2.1 Hz, 1H), 7.34 (dd, J=8.4, 2.1 Hz, 1H), 5.85 (d, J=4.3 Hz, 1H), 3.74 (dd, J=9.7, 3.5 Hz, 1H), 3.21-3.29 (m, 1H), 2.06-2.38 (m, 5H), 1.10-1.88 (m, 10H);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08772500B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-e67a177ad41a4150bdcffe14e9698f5e |
| Source note | uspto-grants-2014_07 |