HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 4-[4-(Acryloyl-methyl-amino)-benzenesulfonyl]-piperazine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(4-Acryloylamino-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 52939519 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-[4-(Acryloyl-methyl-amino)-benzenesulfonyl]-piperazine-1-carboxylic acid tert-butyl ester | HCID 56953731 | 7% |
Reaction Steps
Sodium hydride (0.050 g, 26 mmol) was added in one portion to a stirred solution of 4-(4-acryloylamino-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (0.1 g, 0.25 mmol) in THF (1 ml). The reaction was stirred at room temperature for 5 minutes before methyl iodide (0.05 g, 0.25 mmol) was added in one portion and stirring continued for 1 hour. After this time, the reaction mixture was concentrated under vacuum and the resulting residue purified by prep HPLC to give the title compound (6.6 mg, 7% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946197B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-61f03b82b9ee4000b2828d5b0f441ad1 |
| Source note | uspto-grants-2015_02 |