HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 86717256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | HCID 86717257 | HCID 86717257 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86717256 | HCID 86717256 | — |
Reaction Steps
Excess piperidine was added (0.1 mL, 1 mmol) to a solution of PBD 26 (36.4 mg, 0.03 mmol) in DMF (0.9 mL). The mixture was allowed to stir at room temperature for 20 min, at which point the reaction had gone to completion (as monitored by LC/MS). The reaction mixture was diluted with CH2Cl2 (50 mL) and the organic phase was washed with H2O (3×50 mL) until complete piperidine removal. The organic phase was dried over MgSO4, filtered and excess solvent removed by rotary evaporation under reduced pressure to afford crude product 27 which was used as such in the next step. LC/MS 2.20 min (ES+) m/z (relative intensity) 964 ([M+H]+, 5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09415117B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-a4bb0a9f7e53477b81d3c4e3713c4fb5 |
| Source note | uspto-grants-2016_08 |