Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydride | HCID 166653 | — |
| Reactant | Lithium | HCID 3028194 | — |
| Reactant | HCID 19025023 | HCID 19025023 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19025025 | HCID 19025025 | 83.4% |
Reaction Steps
52.4 g (200 mmol) of ethyl 2-(4-methyl-2-oxo-3-phenyl-3-pyrrolin-1-yl)isobutyrate was dissolved in 300 ml of tetrahydrofuran, and the solution was cooled to -30° C. In a dropping funnel, 7.6 g (200 mmol) of lithium alminum hydride was suspended in 100 ml of tetrahydrofuran, and the suspension was dropwise added at -30° C. After completion of the dropwise addition, the cooling medium was removed, and a suitable amount of water was added, and excess of lithium aluminum hydride was quenched. Insoluble material was removed by filtration, and the filtrate was concentrated and the solid thus obtained was washed with isoproyl ether to obtain 40.9 g (yield: 83%) of the desired product having a melting point of from 77° to 78° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05312929 |
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| Source dataset | uspto-grants-1994_05 |
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| ORD ID | ord-7f8adac5b1c14dccb772c5b78a400617 |
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| Source note | uspto-grants-1994_05 |
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