Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | (2R)-2-{[(tert-butoxy)carbonyl]amino}-3,3-dimethylbutanoic acid | HCID 7005057 | — |
| Reactant | HCID 23138420 | HCID 23138420 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 58858012 | HCID 58858012 | 79% |
Reaction Steps
To a solution of Boc-D-tert-leucine (93 mg) in methylene chloride (2 ml) were added HOBt (81 mg), WSC (114 mg) and triethylamine (0.11 ml) under ice-cooling, and the reaction mixture was mixed at 0° C. for 30 minutes. Then, a solution of 5-methyl-2-(2-(1-piperazinyl)ethyl)-1,2-dihydroimidazo[1,5-c]imidazol-3-one (0.10 g) obtained in Example 97c) in methylene chloride (3 ml) was added, and further mixed at room temperature for 15 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with an aqueous potassium carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified with basic silica gel column (ethyl acetate/methanol=30/1) to obtain the title compound as a colorless oil (0.15 g, 79%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07820673B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-e5c8acbff39e48a8812e9467f035e2f2 |
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| Source note | uspto-grants-2010_10 |
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