Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Glycolic Acid | HCID 757 | — |
| Reactant | Indacaterol | HCID 6918554 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 24178423 | HCID 24178423 | — |
Reaction Steps
A suspension of 2.075 g (R)-5-[2-(5,6-diethyl-indan-2-ylamino)-1-hydroxyethyl]-8-hydroxy-1H-quinolin-2-one base (5.286 mmoles) in 25 ml methanol is heated to 50° C. A solution of 0.402 g glycolic acid (5.286 mmoles) in 5 ml methanol is added dropwise over 7 minutes. The resulting clear solution is stirred at 50° C. Crystallization takes spontaneously place after ca 15 minutes. The white suspension is allowed to cool to room temperature and stirred over night at ca. 25° C. After 18 hours the salt is filtered. The filter cake is washed with 7 ml methanol and dried first 20 hours at 60° C. and ca. 10 mbar and then 2 hours at 60° C. and ca. 1 mbar.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08198450B2 |
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| Source dataset | uspto-grants-2012_06 |
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| ORD ID | ord-4bad1e73354443a6b28a1f42af23013b |
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| Source note | uspto-grants-2012_06 |
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