HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 59750401, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Diethyl chlorophosphate | HCID 13139 | — |
| Reactant | 2-[6-(Aminomethyl)-2-pyridyl]-4h-1,3-benzothiazine-4-one trifluoroacetic acid salt | HCID 68458297 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 59750401 | HCID 59750401 | 55.5% |
Reaction Steps
2-[6-(Aminomethyl)-2-pyridyl]-4H-1,3-benzothiazine-4-one trifluoroacetic acid salt (400 mg, 1.0 mmol) and diethyl chlorophosphate (360 mg, 2.1 mmol) were dissolved in acetonitrile (15 ml), and potassium carbonate (430 mg, 3.1 mmol) was added thereto. The mixture was stirred at room temperature for 15 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-methanol (8:1, v/v) were collected, concentrated and recrystallized from diisopropyl ether-methanol to give the titled compound (225 mg, 53%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07767665B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-826acba591f74b6aa1cdd4bfde9b3e63 |
| Source note | uspto-grants-2010_08 |