HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 76577936, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 76577930 | HCID 76577930 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 76577936 | HCID 76577936 | 70.1% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of 40 (60 mg, 0.15 mmol) in THF/H2O (1:1, 15 ml) LiOH.H2O (30 mg, 0.71 mmol) was added. The mixture was stirred at room temperature and after 2 h 2N HCl was added up to pH=5. The solvent was removed under reduced pressure and a 1:1 mixture of CH2Cl2/MeOH (10 ml) was added. The solution was cooled at 0° C. and the precipitate was collected by filtration, affording 41 (40 mg, 70%) as green solid. 1H NMR (300 MHz, DMSO d6+TFA): δ 8.35 (t, 1H), 8.13 (dd, 1H), 7.91 (m, 2H), 7.78 (ddd, 1H), 4.92 (s, 2H), 3.87 (d, 2H). ESI+MS: calcd for C17H12N6O5: 380.32; found: 381.4 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08648076B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-b9e0d2f3228242f5a9236c42a902e158 |
| Source note | uspto-grants-2014_02 |