HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22321610, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 22321763 | HCID 22321763 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22321610 | HCID 22321610 | 69% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
1-Boc-4-[2-(2-cyanopyridin-4-yl)ethyl]piperazine (4.0 g, 12.64 mmol) was dissolved in methanol (60 mL) and cooled to 0° C. Concentrated hydrochloric acid (10.4 mL, 126 mmol) was added and the mixture stirred for 1 h. The solvents were removed under vacuum and co-evaporated twice with methanol, a 1:1 mixture of methanol/toluene, and finally with methanol. The residue was dried under vacuum overnight to provide crude product (4.5 g). Half of the product was dissolved in methanol, concentrated ammonium hydroxide was added, and solvents were removed under vacuum. The residue was purified by chromatography (SiO2, 100:10:1 CH2Cl2:methanol:concentrated ammonium hydroxide) to provide 1-[2-(2-cyanopyridin-4-yl)ethyl]piperazine (1.05 g, 69%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936611B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-c84b6419e5b240c3bef0444799f8ca41 |
| Source note | uspto-grants-2005_08 |