Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 117667078 | HCID 117667078 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 89709223 | HCID 89709223 | 96.5% |
Reaction Steps
A mixture of 5-(3-aminophenoxy)-3-{[4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-3-methylphenyl]amino}-6-ethylpyrazine-2-carboxamide (840 mg) and 3 M hydrochloric acid (6 mL) was stirred at 80° C. for 5 hours, and then acetic acid (1.5 mL) was added thereto, followed by stirring at 80° C. overnight. The reaction mixture was left to be cooled, and then water (30 mL) was added thereto, followed by ice-cooling. The pH was adjusted to 9 by the addition of concentrated ammonia. The precipitated solid was collected by filtration and then dried under reduced pressure to obtain 5-(3-aminophenoxy)-6-ethyl-3-{[3-methyl-4-(4-oxopiperidin-1-yl)phenyl]amino}pyrazine-2-carboxamide (0.74 g) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09085540B2 |
|---|
| Source dataset | uspto-grants-2015_07 |
|---|
| ORD ID | ord-7bcd44a2e8d646bd83c4730c00109a4b |
|---|
| Source note | uspto-grants-2015_07 |
|---|