HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → HCID 86626336, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 86626335 | HCID 86626335 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86626336 | HCID 86626336 | 84.1% |
Reaction Steps
A solution of 4-fluoro-2-[((S)-2-methoxy-1-methyl-ethyl)-(2,2,2-trifluoro-acetyl)-amino]-benzoic acid tert-butyl ester (2 g, 5.28 mmol) and N-methylpiperazine (5.86 mL, 52.8 mmol) in tetrahydrofuran (20 mL) was stirred at 60° C. for 7 days. The solution was then evaporated, NaHCO3 satured solution was added and the mixture extracted with dichloromethane (3×). The organic layer was washed with water, brine, dried over sodium sulfate filtered and evaporated to obtain a crude, which was purified by column chromatography on silica gel (dichloromethane-methanol 93:7). The title compound (2.04 g, 84%) was obtained as yellowish solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08173659B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-4f4f7d4fdd2b44a4b10a1dbdd096070e |
| Source note | uspto-grants-2012_05 |