HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 56840017, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 56840016 | HCID 56840016 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 56840017 | HCID 56840017 | 61.1% |
Reaction Steps
4-{4-[2-(Tetrahydro-2H-pyran-2-yloxy)ethoxy]piperidin-1-yl}isoquinoline-6-carboxamide (330 mg, 0.83 mmol) produced in Example 19 was dissolved in methanol-water (90:10, V/V, 15 mL), to which p-toluenesulfonic acid monohydrate (213 mg, 1.24 mmol) was then added, followed by stirring at room temperature for 24 hours. After addition of triethylamine (300 μL), the solvent was distilled off under reduced pressure. The residue thus obtained was purified by basic silica gel column chromatography (ethyl acetate:methanol, 100:0-80:20, V/V) to give the desired title compound (160 mg, yield 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685981B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-9539e048e96c4ad98baa65a2cb24face |
| Source note | uspto-grants-2014_04 |