HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperidine → HCID 22312253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 21467080 | HCID 21467080 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22312253 | HCID 22312253 | 48.2% |
Reaction Steps
Piperidine (1.34 g) was added to a solution of crude 5-chloro-1,2-dihydro-1-methyl-3H-1,4-benzodiazepin-2-one hydrochloride (0.005 mol) in dichloromethane (50 ml) cooled in ice. After warming to room temperature, sodium bicarbonate solution (20 ml) was added. The organic phase was separated, dried (Na2SO4) and evaporated to give an orange oil which was purified by column chromatography on silica with CH2Cl2 →CH2Cl2 :MeOH 95:5 as eluant to afford 0.62 g of product as an orange gum 1H NMR (250 MHz, CDCl3) δ: 1.5-1.8 (6H, m), 3.15-3.4 (4H, m), 3.4 (3H, s), 3.5 and 4.25 (2H, ABq, J=11Hz), 7.15-7.6 (5H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05696110 |
| Source dataset | uspto-grants-1997_12 |
| ORD ID | ord-2930de38db6d415da6bf0dd224b70c87 |
| Source note | uspto-grants-1997_12 |