HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 67494869, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| Reactant | (R)-1-Boc-3-methylpiperazine | HCID 2756811 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 67494869 | HCID 67494869 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of 2-chloro-5-nitropyridine (1.0 g, 6.3 mmol), (R)-3-methyl-piperazine-1-carboxylic acid tert-butyl ester (1.4 g, 6.9 mmol) and potassium carbonate (1.308 g, 9.46 mmol) in DMSO (20 mL) was heated at 100° C. overnight. The reaction mixture was cooled to RT, and filtered through a pad of silica gel, eluted with EtOAc (150 mL). The filtrate was washed with water (2×20 mL) and brine (20 mL), dried over sodium sulfate, filtered and concentrated to give a brownish oil which was purified by silica gel chromatography (80 g silica gel, 0-60% EtOAc/hexanes). Desired fractions were combined and concentrated to give the title intermediate as a yellowish solid. (m/z): [M+H]+ calcd for C15H22N4O4 323.16 found 323.3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09260414B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-e0f5e4c9d7654a959a3540251919ad9a |
| Source note | uspto-grants-2016_02 |