Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanolamine | HCID 700 | — |
| Reactant | Trolox | HCID 40634 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67262915 | HCID 67262915 | 49.1% |
Reaction Steps
6-Hydroxy-2,5,7,8-tetramethylchroman-2-carboxylic acid (5.00 g 19.98 mmol) in 150 mL THF was treated with 3.65 g CDI (22.5 mmol) and the exothermic reaction let stir for 1 h at room temperature. Ethanolamine (1.35 g, 22.10 mmol) in 50 mL THF was added over 1 h and the solution stirred overnight. The reaction was concentrated, dissolved into 375 mL CH2Cl2 and washed with 250 mL 0.1 M HCl, 250 mL 0.5 M NaHCO3, 2×100 mL saturated NaCl and dried over Na2SO4. The acidic aqueous phase was extracted 3×100 mL CH2Cl2 and washed with 50 mL saturated NaCl and dried over Na2SO4. The combined organics were concentrated and purified by flash chromatography yielding 2.88 g of 6-hydroxy-N-(2-hydroxyethyl)-2,5,7,8-tetramethylchroman-2-carboxamide as an off white impure solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08519001B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-4fa109a9aad54244aea63b08dbc48916 |
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| Source note | uspto-grants-2013_08 |
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