HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 42643627, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| 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 59542561 | HCID 59542561 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 42643627 | HCID 42643627 | 42.5% |
Reaction Steps
2-Chloro-5-ethyl-thiophene-3-carboxylic acid (0.04 g, 0.21 mmol) was dissolved in DMF (6 mL). DIPEA (0.63 mmol), HATU (0.21 mmol) and piperidine (2.0 mmol) were added and the reaction stirred overnight. The mixture was diluted with acetonitrile and water and the product purified by HPLC, eluting with 20%-95% 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 (0.023 g). LCMS m/z 358.08 [M+H]+RT=10.84 min (Analytical Method 2). 1H NMR (400 MHz, CHCl3-d): δ 6.6 (s, 1H), 3.7 (s, 2H), 3.35 (s, 2H), 2.75 (q, 2H), 1.6 (s, 6H), 1.3 (t, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362008B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-c74d3a3caa924cbca4385dc1639a83c9 |
| Source note | uspto-grants-2013_01 |