HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1'-Carbonyldiimidazole → Tert-butyl 4-(2-oxo-1,2,4,5-tetrahydrobenzo[d][1,3]diazepin-3-yl)piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | Tert-butyl 4-{[2-(2-aminophenyl)ethyl]amino}piperidine-1-carboxylate | HCID 18444264 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Tert-butyl 4-(2-oxo-1,2,4,5-tetrahydrobenzo[d][1,3]diazepin-3-yl)piperidine-1-carboxylate | HCID 58823744 | — |
Reaction Steps
To a solution of tert-butyl 4-(2-aminophenethylamino)piperidine-1-carboxylate (6.9 g, 30 mmol) in DMF (110 ml) was added CDI (4.86 g, 30 mmol) in portions followed by stirring the reaction mixture at RT for 2 h. The reaction mixture was diluted with water and extracted with EtOAc. The organics were combined, washed with water, brine, and evaporated to dryness to give the desired product. LC/MS (10% to 99%): M/Z (M+H)+ (obs)=346; tR=3.24.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163737B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-46696c2d8d464311ae5b4e984caf4a13 |
| Source note | uspto-grants-2012_04 |