HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylpiperidine-1-carbonyl Chloride → HCID 11608827, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylpiperidine-1-carbonyl Chloride | HCID 15221516 | — |
| Reactant | HCID 178518958 | HCID 178518958 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 11608827 | HCID 11608827 | — |
Reaction Steps
100 mg (0.66 mmol) of 4-fluoro-1H-indazol-3-ol and 116.8 mg (0.72 mmol) of 4-methylpiperidine-1-carbonyl chloride (Example 2) in 10 ml of pyridine were heated under reflux for 4 h and left to stand overnight. Addition of 24 mg of 4-methyl-piperidine-1-carbonyl chloride was followed by heating under reflux for a further 2 h while the pyridine was distilled off in vacuo, and the residue was dissolved in water and extracted with ethyl acetate. The organic phase was concentrated and purified by preparative HPLC (PR18, acetonitrile/water 0.1% TFA). Yield: 56 mg (31%), M+H+: 278.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07528155B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-e8f003b8843547d280f5e1beb62d127b |
| Source note | uspto-grants-2009_05 |