HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 58786412, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,1-Dimethylethyl 4-[2-amino-1-(2-fluorophenyl)ethyl]-1-piperazinecarboxylate | HCID 58786464 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58786412 | HCID 58786412 | 98% |
Reaction Steps
To a solution of 4-[2-Amino-1-(2fluoro-phenyl)-ethyl]-piperazine-1-carboxylic acid tert-butyl ester (207) (0.71 g, 2.19 mmol) in THF (5 mL) at 0° C. was added diisopropylethylamine (0.42 mL, 2.42 mmol). The solution was allowed to stir for 10 min. Methansulfonyl chloride (0.17 mL, 2.19 mmol) was then added and the solution was allowed to stir at room temperature for 18 h. The reaction mixture was diluted with EtOAc (50 mL) and washed with brine (50 mL) and H2O (50 mL). The organic phase was concentrated to dryness yielding 0.86 g (98%) product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07169777B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-9c9b8a3ace3247218fccfc3a8f15bd8b |
| Source note | uspto-grants-2007_01 |