Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| Reactant | HCID 11227728 | HCID 11227728 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 87605692 | HCID 87605692 | 86.3% |
Reaction Steps
A mixture of (2E)-3-{3-[7-chloro-3-(2-{[4-fluoro-2-(trifluoromethyl)phenyl]amino}-2-oxoethyl)-6-methyl-2-oxo-2H-chromen-4-yl]phenyl}acrylic acid (10.0 g), tris(hydroxymethyl)methylamine (2.2 g), ethanol (70 ml) and acetonitrile (100 ml) was heated and stirred at 70° C. to dissolve the mixture. Acetonitrile (200 ml) was slowly added to the reaction mixture, and the mixture was stirred at 70° C. for 3 hours, gradually cooled to room temperature, and then stirred at room temperature overnight. Crystals obtained were collected by filtration, washed with acetonitrile, and dried at 60° C. for 8 hours under reduced pressure to obtain the title compound as colorless crystals (10.5 g, yield 86%). The crystals obtained showed the X-ray powder diffraction pattern as shown in FIG. 3 and crystallinity was 64%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07541478B2 |
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| Source dataset | uspto-grants-2009_06 |
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| ORD ID | ord-5c1f0527f0ed43b19d8bee4ea65582cc |
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| Source note | uspto-grants-2009_06 |
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