Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Chloride | HCID 433294 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 68680027 | HCID 68680027 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 59516008 | HCID 59516008 | 44% |
Reaction Steps
A mixture of sodium borohydride (3.7 g, 98 mmol) and lithium chloride (4.2 g, 101 mmol) in ethanol (70 ml) was stirred at 5° C. for 15 min, 9H-fluorene-2,7-diacrylic acid dimethyl ester (5.0 g, 15 mmol) in diglyme (150 ml) was added portionwise at 20-50° C. and the mixture was refluxed for 18 h. Diluted hydrochloric acid was added dropwise after cooling and the mixture was extracted with diethyl ether. Organic layer was separated, dried (MgSO4) and evaporated to give a residue, which was purified by chromatography on silica gel. Elution with ethyl acetate afforded 1.85 g (44%) of the title compound as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07816385B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-aa5a105edcc747da9d0cfa7c6baf6e3f |
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| Source note | uspto-grants-2010_10 |
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