HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine → HCID 21104165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 21103673 | HCID 21103673 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21104165 | HCID 21104165 | 59.9% |
Reaction Steps
Compound 39 (470 mg, 1 mmol) was dissolved in MeOH (15 mL) and THF (15 mL). Raney Nickel (50% slurry in water) (2 mL) was added to the reaction mixture followed by anhydrous hydrazine (1 mL). The reaction mixture was stirred at room temperature for 30 minutes until the bubbling was stopped. The solid was filtered off through Celite under reduced pressure and washed with MeOH. The solvent was removed under reduced pressure. Liquid-liquid extraction was performed using CHCl3 (15 mL) and H2O (8 mL×2). The organic layer was dried over MgSO4, filtered and concentrated to give the compound 40 (263.8 mg, 59.9% crude yield) LC-MS (ESI): m/e=441.1 [M+1]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07223759B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-9d490996b5764c038fde2d1df3de17c0 |
| Source note | uspto-grants-2007_05 |