Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 69702056 | HCID 69702056 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 69710152 | HCID 69710152 | 18% |
Reaction Steps
To a solution of the product from Step B (2.90 g, 6.18 mmol) in anhydrous 1-methyl-2-pyrrolidone (30 mL) was added sodium hydride (60%, 0.371 g, 9.27 mmol). The mixture was heated at 50° C. overnight and at ambient temperature for 2 days, cooled and poured into a saturated aqueous solution of sodium bicarbonate (100 mL) and extracted with ethyl acetate. Chromatography on silica (gradient, 2% to 25% ethyl acetate in hexane) gave an oil (0.48 g, 18%): LC/MS (+APCI) m/z 433(M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06696476B2 |
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| Source dataset | uspto-grants-2004_02 |
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| ORD ID | ord-385b5b8d900c4a34aaff49055a0097b3 |
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| Source note | uspto-grants-2004_02 |
|---|