HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azepane → HCID 59542474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azepane | HCID 8119 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| Reactant | HCID 59542569 | HCID 59542569 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59542474 | HCID 59542474 | 70.1% |
Reaction Steps
3-(4-Carboxy-thiophen-2-yl)-piperidine-1-carboxylic acid tert-butyl ester (0.075 g, 0.24 mmol) was dissolved in DMF (2 mL). Triethylamine (0.72 mmol), HATU (0.26 mmol) and homopiperidine (0.26 mmol) were added and the reaction stirred at room temperature overnight. The reaction mixture was purified directly by HPLC, eluting with 10%-98% acetonitrile in water (0.1% formic acid) over 30 minutes. The fractions containing the desired product were concentrated under vacuum to give the title compound (0.066 g). LCMS m/z 393.26 [M+H]+ RT=4.05 min (Analytical Method 4).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362008B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-95a6948465794665ad742dc75919db7d |
| Source note | uspto-grants-2013_01 |