HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → Tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate | HCID 15829156 | 78% |
Reaction Steps
Piperazine-1-carboxylic acid tert-butyl ester (3.0 g, 16.1 mmol) and DIPEA (3.1 ml, 18.0 mmol) were dissolved in DCM (32 ml) and cooled in ice bath. To the above stirred mixture was added a solution of chloroacetyl chloride (1.33 ml, 16.7 mmol) at 0° C. Three hours later, the mixture was washed with water, dried and evaporated under reduced pressure. The residue was purified by column chromatography using EA/PE (4/1) as eluent to afford the title compound (3.3 g, yield 78.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431581B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-fc146c13c4bb4c81a36b35ad43655081 |
| Source note | uspto-grants-2013_04 |