HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → HCID 89739210, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Tert-butyl 4-(6-aminopyridin-2-yl)piperazine-1-carboxylate | HCID 50986448 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 89739210 | HCID 89739210 | 8.2% |
Reaction Steps
To a solution of tert-butyl 4-(6-aminopyridin-2-yl)piperazine-1-carboxylate (1.9 g, 8 mmol) in N,N-dimethylformamide (20 ml) was added dropwise 1-bromopyrrolidine-2,5-dione (1.4 g, 8 mmol) at 0° C. The reaction was allowed to stirred for 4 h at rt. The reaction mixture was quenched with water (30 mL), and extracted with acetic ester (30 mL×3). The combined organic phase was dried by anhydrous sodium sulphate, and then filtered. The filtrate was concentrated and purified by column chromatograph silica gel (elute: petroleum ether/ethyl acetate=1:1) to give tert-butyl 4-(6-amino-5-bromopyridin-2-yl)piperazine-1-carboxylate (0.2 g, 8.2%) as a yellow solid. LCMS (M+H) m/z: calcd. 356.08. found 357.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09371331B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-d2b9ba550d2b48b7b5d9eb70216bb8d2 |
| Source note | uspto-grants-2016_06 |