HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 68433229, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2-{4-[(E)-3-(3,4-Dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-ylmethyl}-acrylic acid ethyl ester | HCID 68434870 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68433229 | HCID 68433229 | 44.8% |
Reaction Steps
A suspension of 0.80 g (1.88 mmol) of 2-{4-[(E)-3-(3,4-dichloro-phenyl)-acryloyl]-7-oxo-[1,4]diazepan-1-ylmethyl}-acrylic acid ethyl ester, 0.56 ml (5.64 mmol) of piperidine and 1.83 g (5.61 mmol) of cesium carbonate in 32 ml of acetonitrile was stirred over night at RT. Additional 0.37 ml (3.76 mmol) of piperidine were added and after 1 h, cesium carbonate was filtrated and the solvent evaporated. Purification by flash silica gel column (CH2Cl2/MeOH 98:2 to 96:4) gave 0.43 g (44%) of the title compound as colorless foam. MS: 510.4 (MH+, 2Cl).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07632829B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-59856de9f17448f2bbb374caf509331c |
| Source note | uspto-grants-2009_12 |