HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Bromoacetyl bromide | HCID 61147 | — |
| Reactant | tert-Butyl 4-(6-aminopyrimidin-4-yl)piperazine-1-carboxylate | HCID 21934614 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate | HCID 15829155 | — |
Reaction Steps
A solution of bromoacetyl bromide (0.59 g, 2.95 mmol) in methylene chloride (3 mL) was added drop wise via addition funnel to a stirred solution of tert-butyl piperazine-1-carboxylate 12-1 (0.50 g, 2.68 mmol) and aqueous sodium carbonate (0.34 g, 3.22 mmol) in methylene chloride (15 mL) at 0° C. After a 10 minute reaction time the methylene chloride layer was drawn off, dried and evaporated to an oil. This was purified this on a silica column to afford 42-1. Hi-Res MS (M+Na): calc: 329.0471 found: 329.0462. 1H-NMR(CDCl3): 3.87(s, 2H); 3.61(m, 2H); 3.52(m, 2H); 3.50(m, 2H); 3.44(m, 2H); 1.47(s, 9H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115597B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-06e41ac235554e3a94252187fedbbc85 |
| Source note | uspto-grants-2006_10 |