Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | HCID 70976343 | HCID 70976343 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68272223 | HCID 68272223 | 52% |
Reaction Steps
A mixed liquid containing LiCl (0.175 g, 4 mmol), ethyl 2,2-bis(4-bromobenzyl)-3-oxobutanoate (0.94 g, 2 mmol) and H2O (0.036 mL) in DMF (4 mL) was stirred under heating at 120° C. for 48 hours. The mixed liquid was then cooled to room temperature, water (10 mL) was added, and the resulting mixture was extracted with ethyl acetate. The resulting organic layer was washed with a saturated saline solution and then dried using MgSO4. The organic layer was concentrated under reduced pressure, and then purified using silica gel column chromatography, yielding the title compound (41) in a yield of 52%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09051246B2 |
|---|
| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-3be31b9f245c4d1ba6df064e677ba663 |
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| Source note | uspto-grants-2015_06 |
|---|