HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azepane → HCID 42646245, 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 | 13191-44-1 | HCID 59542503 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 42646245 | HCID 42646245 | 53.9% |
Reaction Steps
5-(Cyclohexyl)-thiophene-3-carboxylic acid (0.03 g, 0.14 mmol) was dissolved in acetonitrile (2 mL). Triethylamine (0.42 mmol), HATU (0.15 mmol) and azepane (0.14 mmol) were added and the reaction stirred at room temperature overnight. The resulting solution 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 (0.022 g). LCMS m/z 292.22 [M+H]+ RT=13.57 min (Analytical Method 1). 1H NMR δ (ppm) (CHCl3-d): 7.2 (s, 1H), 6.95 (s, 1H), 3.7-3.4 (m, 4H), 2.8 (m, 1H), 2.1 (m, 2H), 1.9-1.2 (m, 16H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362008B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-09c0d99a1d314cf49cac836cb38a62e3 |
| Source note | uspto-grants-2013_01 |