HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 57494065, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | Piperazine-2-carboxylic acid dihydrochloride | HCID 2723757 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 57494065 | HCID 57494065 | — |
Reaction Steps
To a suspension of piperazine-2-carboxylic acid dihydrochloride (10 g) in 1,4-dioxane (100 mL) and water (50 mL) at 0° C. was added 17M NaOH solution in portions followed by di-tert-butyldicarbonate (11.8 g). The resulting mixture was warmed to R.T. and stirred for 5 h. Triethylamine (13.7 mL) and methanesulfonyl chloride (3.8 mL) were added this mixture was stirred overnight at R.T. The reaction mixture was concentrated in vacuo, diluted with 2M HCl and extracted with EtOAC. Combined extracts were dried (MgSO4), filtered and concentrated to give 4-methanesulfonyl-piperazine-1,3-dicarboxylic acid 1-tert-butyl ester (8.46 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802670B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-37ecc69abe114624b73cf485110ba095 |
| Source note | uspto-grants-2014_08 |