Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetaldehyde | HCID 177 | — |
| Reactant | Phthalide | HCID 6885 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57457555 | HCID 57457555 | 49.1% |
Reaction Steps
A dry tetrahydrofuran solution (100 mL) of lithium diisopropyl amide (26.9 mmol) was cooled to −78 degree in a current of nitrogen, and a tetrahydrofuran solution (100 mL) of phthalide (3.0 g, 22.4 mmol) was dripped in. After stirring at −78° C. for 30 minutes, acetaldehyde (1.19 g, 26.9 mmol) was slowly added and stirred at −50° C. for 4 hours. After the temperature had risen to room temperature, distilled water was added and the mixture extracted with ethyl acetate. The organic phase was washed with distilled water and saturated brine, and dried with anhydrous sodium sulfate. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/6), and the target compound (1.96 g, 49%) was obtained as a yellow oily residue.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08268842B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-6c88743586254ec4b1a29f464ee22971 |
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| Source note | uspto-grants-2012_09 |
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