HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methyl-2-pyrrolidone → HCID 68312323, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | 4,4-Difluoropiperidine hydrochloride | HCID 2758351 | — |
| Reactant | 2-Chloro-5-fluoro-4-methylpyrimidine | HCID 20778073 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68312323 | HCID 68312323 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A 5 mL microwave vial was charged with 2-chloro-5-fluoro-4-methylpyrimidine (JOC 2004, 69, 3943-3949) (0.19 g, 1.3 mmol), 4,4-difluoropiperidine hydrochloride (1.0 g, 6.5 mmol) and NMP (2.6 mL). The mixture was heated in a microwave oven at 120° C. for 24 hours then cooled to ambient temperature. The mixture was then diluted with EtOAc, washed with water (3×), and brine. The organic extract was concentrated and purified by chromatography (silica gel, 0-5% EtOAc/hexanes gradient) to afford the title compound. MS (ESI) m/z: 232.4 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09012651B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-d706012f0e324377b061e223dc06000b |
| Source note | uspto-grants-2015_04 |