HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 22272508, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 22272427 | HCID 22272427 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Tetrahydrofuran ethanol | HCID 21873804 | — |
| Product | HCID 22272508 | HCID 22272508 | 93.4% |
Reaction Steps
To a solution of tert-butyl 4-[3-(ethylamino)-4-nitrophenyl]-1-piperazinecarboxylate (1.028 g, 2.93 mmol) in 40 mL EtOH:THF (4:1) solvent system was added Raney-Ni (1 mL of a EtOH suspension) followed by addition hydrazine hydrate (0.734 g, 14.67 mmol). The mixture was stirred vigorously for 3 hours and then filtered through a Celite pad pretreated with water. The filtrate was concentrated and then purified by column chromatography on silica using CHCl3/MeOH/NH3 9:1:0.4% as eluent to give 0.877 g (93%) of a red oil. The oil was used immediately in the next reaction. HPLC purity>90%; MS (posEI) m/z=320 (M+);
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07718650B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-d515745fee20413dbf60db88657cf4b9 |
| Source note | uspto-grants-2010_05 |