Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | Indacaterol | HCID 6918554 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 1000160-87-1 | HCID 10255695 | — |
Reaction Steps
A suspension of 2.208 g (R)-5-[2-(5,6-diethyl-indan-2-ylamino)-1-hydroxyethyl]-8-hydroxy-1H-quinolin-2-one base (5.625 mmoles) in 20 ml methanol is heated to 50° C. A solution of 0.326 g fumaric acid (2.81 mmoles) in 5 ml methanol is dropwise added to the suspension at constant flow rate, over 10 minutes. The resulting solution is stirred at 50° C. Crystallization takes then spontaneously place after ca. 10 minutes. The suspension is allowed to cool and stirred for 3 hours at room temperature. The mixture is filtered. The crystals are washed with 7 ml methanol and dried first for 20 hours at 60° C. and ca. 10 mbar and further for 2 h at 60° C. and ca. 1 mbar. Yield: 2.19 g white powder (86.4%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08198450B2 |
|---|
| Source dataset | uspto-grants-2012_06 |
|---|
| ORD ID | ord-7ffa1c8d1106486fb84b59d6ef2ef108 |
|---|
| Source note | uspto-grants-2012_06 |
|---|