HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 68183192, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68183006 | HCID 68183006 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | MeOH tetrahydrofuran | HCID 21899815 | — |
| Product | HCID 68183192 | HCID 68183192 | 17.2% |
Reaction Steps
LiOH (10 mg, 0.25 mmol) in water (0.5 ml) was added to a solution of 2-fluoro-5-(2-methyl-3,3-dioxo-1,2,3,4-tetrahydro-3λ*6*-thia-2,4,5-triaza-phenanthren-1-yl)-benzoic acid methyl ester 423 (50 mg, 0.12 mmol) in THF:MeOH (1:1; 2 ml) and the mixture was stirred at room temperature for 1 h. The mixture was concentrated in vacuo, the residue was diluted in the minimum amount of water and acidified to pH=3-4 with 2 M HCl. The resulting precipitate was collected by filtration and dried. The crude solid was purified by preparative HPLC (acidic conditions 1) to give the title compound (8 mg, 17%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09102688B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-60255a85d88242c397d41fca615bf15b |
| Source note | uspto-grants-2015_08 |