Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 17825670 | HCID 17825670 | — |
| Reactant | HCID 86590786 | HCID 86590786 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 69075956 | HCID 69075956 | — |
Reaction Steps
355 mg (1.20 mmol) of acetoacetic acid 3,3-diphenylpropyl ester and 277 mg (3.59 mmol) of ammonium acetate were stirred in 15 ml of 2-propanol at 55° C. overnight. After evaporating 2-propanol under reduced pressure, ethyl acetate was added and the reaction mixture was washed with saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The obtained substance was dissolved in 15 ml of 2-propanol. 513 mg (1.20 mmol) of 4-[2-acetyl-3-(3,5-dichlorophenyl)-2-propenoyl] piperazine-1-carboxylic acid-t-butyl ester was added and stirred at 70° C. overnight. After evaporating 2-propanol under reduced pressure, the residue was purified by the silica gel chromatography (dichloromethane/methanol=100/1 to 50/1) to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07494989B2 |
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| Source dataset | uspto-grants-2009_02 |
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| ORD ID | ord-b0a036cae11b43a8a4435207af29b9e7 |
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| Source note | uspto-grants-2009_02 |
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