Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178471952 | HCID 178471952 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 131723021 | HCID 131723021 | 84.2% |
Reaction Steps
45 mg of sodium hydride (abt. 60% oil suspension 1.13 mmol) was added to 5 ml of a tetrahydrofuran solution of 411 mg of the compound obtained in Example 1 (1.08 mmol) under an argon atmosphere at 0° C. and the solution was stirred at the same temperature for 5 minutes. It was further stirred at room temperature for 30 minutes, then water (15 ml) was added and extraction was performed with ethyl acetate (30 ml). Next, the organic layer was washed with saturated saline (10 ml), then dried over anhydrous sodium sulfate, then the solvent was distilled off under vacuum. The precipitated crystal was washed with diethyl ether and the crystal was obtained by filtration to obtain 314 mg (84%) of the above-identified compound as a colorless crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06331548B1 |
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| Source dataset | uspto-grants-2001_12 |
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| ORD ID | ord-acb23c9d6b29451696d16c91c7c89bdf |
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| Source note | uspto-grants-2001_12 |
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