HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69108009, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86590779 | HCID 86590779 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69108009 | HCID 69108009 | 88.6% |
Reaction Steps
A 40 ml portion of 1 N sodium hydroxide aqueous solution was added dropwise to 40 ml of THF solution containing 3.36 g of ethyl (2R,5S)-4-{[4-(4-cyano-3-trifluoromethylphenyl)-2,5-dimethylpiperazine-1-carbonyl]amino}pyridine-2-carboxylate synthesized in Example 18-3, and the mixture was stirred at room temperature for 1 hour. This was adjusted to pH 2 to 3 by adding 4 N hydrochloric acid under ice-cooling, and the thus formed precipitate was collected by filtration, washed with purified water and then dried at 70° C. under reduced pressure to obtain 2.80 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06673799B1 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-94e5447c32a743fa81c0c4e09ab7b334 |
| Source note | uspto-grants-2004_01 |