Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 70049909 | HCID 70049909 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70047968 | HCID 70047968 | 48% |
Reaction Steps
10 ml of 1M borane/THF complex was added to 10 ml of a solution of 0.81 g (2.6 mmol) of trans-3-benzyl-4-(3,4-dimethoxyphenyl)-2-pyrrolidone in THF, and the mixture was heated under reflux for 6 hr. After the completion of the cooling, 10 ml of a 6N hydrochloric acid solution was dropwise added at room temperature carefully, and the mixture was stirred at 60° C. for 30 min. THF was distilled off in vacuo, and the residue was basified with a 10% aqueous sodium hydroxide solution and extracted twice with methylene chloride. The resultant organic phase was dried over anhydrous sodium sulfate, and the solvent was distilled off in vacuo to prepare a crude product. The crude product was adsorbed on silica gel to elute impurities (methylene:methanol=95:5), and elution was again conducted to prepare 0.37 g (yield: 48%) of an intended product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05444083 |
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| Source dataset | uspto-grants-1995_08 |
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| ORD ID | ord-97b758ff035d48cd9c77ebdd17598fdf |
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| Source note | uspto-grants-1995_08 |
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