HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylpiperidine → HCID 58211669, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylpiperidine | HCID 69381 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 6-Bromopyridine-2-carboxylic acid | HCID 593919 | — |
| Reactant | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58211669 | HCID 58211669 | 97% |
Reaction Steps
After 6-bromopicolinic acid (500 mg, 2.48 mmol) was suspended in acetonitrile (25 ml), 4-methylpiperidine (0.44 ml, 3.72 mmol), N,N-diisopropylethylamine (0.65 ml, 3.72 mmol), and HBTU (1.13 g, 2.97 mmol) were sequentially added thereto, and then the resulting mixture was stirred at room temperature under nitrogen stream for 4 hours. The resulting reaction liquid was concentrated under reduced pressure, and then the residue thus obtained was subjected to MPLC (30% EtOAc/Hexanes), to obtain 677 mg of white solid (97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096571B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-20ae218e56da4474b454d430b7b122fe |
| Source note | uspto-grants-2015_08 |