HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 1,4-Di-tert-butyl 2-methyl piperazine-1,2,4-tricarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1,4-Di-Boc-piperazine-2-carboxylic acid | HCID 11255979 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1,4-Di-tert-butyl 2-methyl piperazine-1,2,4-tricarboxylate | HCID 22458573 | 90% |
Reaction Steps
To a solution of 1,4-bis(tert-butoxycarbonyl)piperazine-2-carboxylic acid (2.5 g, 7.56 mol) in acetonitrile (25 mL) was Cs2CO3 (3.93 g, 12.06 mol) with stirring at RT. After 15 min, MeI (2.34 g, 16.48 mol) was added. The reaction mixture was stirred at rt for 14 h. The reaction was monitored by TLC. When SM was finished, reaction mixture was filtered through celite pad and filtrate was concentrated. Column chromatography of crude material afforded product 1,4-di-tert-butyl 2-methyl piperazine-1,2,4-tricarboxylate (29) as white solid (2.35 g, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238656B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-5292509452e84d10aee2ad6969b627be |
| Source note | uspto-grants-2016_01 |