Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 68322495 | HCID 68322495 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 53241610 | HCID 53241610 | 12.6% |
Reaction Steps
A mixture of N-[({4-[(3-chloro-4-fluorophenyl)oxy]phenyl}amino)carbonyl]-D-alanine (Intermediate 9, 352 mg) in 15 mL of 3N HCl was heated at 100° C. for 16 hours. Then sodium carbonate was added and the mixture was adjusted to pH=8. The mixture was extracted with ethyl acetate (3 times 50 mL) and the combined organic phases were washed with brine and dried over magnesium sulphate. Removal of the solvent afforded a residue which was purified by column chromatography (MeOH/DCM=1/50) to give 42 mg of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09216967B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-088db794c30f45be981712932d88e79f |
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| Source note | uspto-grants-2015_12 |
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