Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-Iodopropane | HCID 33643 | — |
| Reactant | HCID 67103490 | HCID 67103490 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67103581 | HCID 67103581 | — |
Reaction Steps
The compound (961 mg) obtained in Example 48-1 was dissolved in DMF (20 ml). After having been cooled to 0° C., the solution was added with 60% sodium hydride (72.9 mg) and warmed back to room temperature and the whole was stirred for 30 minutes. 1-Iodopropane (0.30 ml) was dropped to the solution and the whole was stirred for additional 3 hours. After having been cooled to 0° C., the solution was added with water to stop the reaction and concentrated. The residue was subjected to extraction with chloroform. The organic layer was washed with water and a saturated saline solution, and dried with anhydrous sodium sulfate. The residue obtained by distilling the solvent off was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (317 mg) as a yellow oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07932281B2 |
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| Source dataset | uspto-grants-2011_04 |
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| ORD ID | ord-eb11a9c382454cfaa089a08b195217fc |
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| Source note | uspto-grants-2011_04 |
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