Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-[[Bis(allyloxy)phosphoryl]oxy]-2,2-dimethylbutyl chloride | HCID 21110462 | — |
| Reactant | HCID 178462432 | HCID 178462432 | — |
| Product | HCID 178460585 | HCID 178460585 | 15% |
Reaction Steps
According to a similar procedure to that described in Example 1-(12), 4-[(1E,3E)-4-[trans-5-[[(1R,2R)-2-(2,4-difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]thio]-1,3-dioxan-2-yl]-1,3-butadienyl]-3-fluorobenzonitrile (1.09 g, 2.0 mmol) described in Reference example 1, sodium hydride (55% dispersion in mineral oil; 104.7 mg, 2.4 mmol), and 4-[[bis(allyloxy)phosphoryl]oxy]-2,2-dimethylbutyl chloride were reacted in tetrahydrofuran (10 ml) and the reaction mixture was worked up to afford, after extraction, the title compound as a crude oil. The crude oily product was subjected to chromatography on a silica gel (75 g) column (eluent; ethyl acetate:hexane=2:1˜3:1) to afford the title compound (238.8 mg, 15% yield) as a pale yellow amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07230023B2 |
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| Source dataset | uspto-grants-2007_06 |
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| ORD ID | ord-dcac95bd96cd43f6a24bca426b983a16 |
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| Source note | uspto-grants-2007_06 |
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