Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | 4-(2-ethyl-1,3-dioxan-2-yl)-2-methoxypyridine | HCID 10846732 | — |
| Reactant | Tmsci | HCID 131723440 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 22987177 | HCID 22987177 | — |
Reaction Steps
A mixture of 4-(2-ethyl-1,3-dioxan-2-yl)-2-methoxypyridine (prepared according to the method described in the Patent Application PCT/FR96/00980, 57 g, 255 mmol) and sodium iodide (88 g, 580 mmol) in acetonitrile (1 l) is treated with trimethylsilane chloride (74 ml, 586 mmol), taken to reflux for 3 hours, then agitated at ambient temperature for 16 hours. The reaction medium is then treated with water (100 ml) and concentrated to dryness after elimination of the insolubles by filtration. The residue is taken up in ethyl acetate and washed successively with water and with an aqueous solution saturated in sodium chloride. The organic phase is dried, concentrated under reduced pressure, and the residue is taken up in diethyl ether in order to produce after filtration and drying 30 g (88%) of a white solid, m.p. 168° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06436951B1 |
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| Source dataset | uspto-grants-2002_08 |
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| ORD ID | ord-2aa2302fcdb44fa1904cf5181edeabc2 |
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| Source note | uspto-grants-2002_08 |
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