HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 86271573, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 90418066 | HCID 90418066 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 86271573 | HCID 86271573 | — |
Reaction Steps
To a solution of Example 86A (266 mg, 0.556 mmol) in 4 mL of tetrahydrofuran/water (3:1) was added lithium hydroxide mono hydrate (46.7 mg, 1.112 mmol). The reaction was stirred at room temperature overnight. The volatiles were then removed, and the residue dissolved in 5 mL water and the pH was adjusted to pH ˜6-7 with 1 M hydrochloric acid. The solid was collected by filtration and dried under high vacuum overnight to give the title compound as a hydrochloride salt. 1H NMR (400 MHz, DMSO-d6) δ 12.26 (s, 1H) 8.81 (s, 1H) 7.13-7.52 (m, 3H) 6.62 (s, 1H) 6.32 (s, 1H) 3.83 (s, 3H) 3.32 (d, J=21.06 Hz, 2H) 2.67-2.86 (m, 2H) 2.56 (s, 1H) 2.41 (s, 1H) 2.10-2.27 (m, 1H) 1.83-2.08 (m, 3H) 1.24-1.76 (m, 6H). MS (ESI+) m/z 451.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346813B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-3b2331320107430cae69d2cb02af68fe |
| Source note | uspto-grants-2016_05 |