Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 86657596 | HCID 86657596 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67389658 | HCID 67389658 | 62.6% |
Reaction Steps
(R)-5-(4-Cyano-benzyl)-7-(3,5-dichloro-phenyl)-5-methyl-6-oxo-6,7-dihydro-5H-imidazo[1,2-a]imidazole-3-carboxylic acid {1-[1-(4-aminomethyl-pyridin-2-yl)-cyclopropylcarbamoyl]-cyclopropyl}-amide dihydrochloric acid salt (40 mg, 0.0539 mmol) was suspended in DCM (1 mL). TEA (0.038 mL, 0.269 mmol) was then added and the reaction mixture became homogeneous. Acetic anhydride (0.00624 mL, 0.0646 mmol) was then added. Stirred for 5 min. Solvent was evaporated. The resultant crude product was purified by reverse phase HPLC using 30-100% ACN/water as the gradient. Solvent was evaporated. The product was redissolved in 10% MeOH/DCM and filtered through a basic (NH2) cartridge. Solvent was evaporated to afford 24 mg of the title compound as a white solid, m/z 711.7 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08552205B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-281f1e305ee14eaf9fc0a33007d31e19 |
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| Source note | uspto-grants-2013_10 |
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