HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloropyrimidine → 3,5-Dimethyl-4-pyrimidin-2-ylpiperazine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloropyrimidine | HCID 74404 | — |
| Reactant | Tert-butyl 3,5-dimethylpiperazine-1-carboxylate | HCID 22219990 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3,5-Dimethyl-4-pyrimidin-2-ylpiperazine-1-carboxylic acid tert-butyl ester | HCID 59406986 | 18.2% |
Reaction Steps
3,5-Dimethylpiperazine-1-carboxylic acid tert-butyl ester (1.676 g) and 2-chloropyrimidine (716 mg) were combined, melted in an oil bath at 120° C., and stirred for 5 hr 30 min. Water (10 ml) was added and the mixture was stirred, extracted with ethyl acetate (30 ml), and washed with saturated brine. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated. The obtained residue was purified by column chromatography (Yamazen HI-FLASH™ COLUMN size L, elution solvent: hexane/ethyl acetate) to give the title compound (333 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835631B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-cd96fb9f93694b3db7b4bb7b950145d4 |
| Source note | uspto-grants-2014_09 |