Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 66645513 | HCID 66645513 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66645676 | HCID 66645676 | 53% |
Reaction Steps
11.19 g of cesium carbonate (34.4 mmol) was added to a solution of 4.41 g of {2-[(2-bromoacetyl)phenylamino]-1,1-dimethylethyl}carbamic acid t-butyl ester obtained in the above reaction (11.5 mmol) in N,N-dimethylformamide (58 ml) under ice-cooling, and the mixture was stirred at room temperature for 18 hours. Water was added to the reaction mixture, followed by extraction with ethyl acetate. Then, the organic layer was washed with water and brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:hexane/ethyl acetate=10/1-5/1-2/1) to obtain 1.83 g of 2,2-dimethyl-5-oxo-4-phenylpiperazine-1-carboxylic acid t-butyl ester (yield: 53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08158790B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-a78b112aaf264572b73911a0c78ede0d |
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| Source note | uspto-grants-2012_04 |
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