HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl 4-(3-nitropyridin-2-yl)piperazine-1-carboxylate → HCID 21477686, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl 4-(3-nitropyridin-2-yl)piperazine-1-carboxylate | HCID 21477687 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 21477686 | HCID 21477686 | — |
Reaction Steps
1-[Benzyloxycarbonyl]-4-[3-nitro-2-pyridinyl]piperazine (PREPARATION 32), is dissolved in dioxane (923 ml) and cooled to 0°. Then aqueous titanium trichloride (20%, 555.3 ml) is added cautiously. After stirring 30 min the reaction is diluted with aqueous sodium hydroxide solution (2N, 1.5 l) and filtered through celite. The filter cake is washed with methanol/chloroform (10/90). The combined organic layers are washed with water, saline, dried and concentrated in vacuo to afford the desired product, NMR (300 MHz, CDCl3) 7.80, 7.38-7.32, 6.99, 6.88, 5.17, 3.67 and 3.12 δ.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05686610 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-5b2a8864e2f344809372c112a7a9af95 |
| Source note | uspto-grants-1997_11 |