関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Iodomethyl-5-ethyl-2-(3-methoxyphenyl)oxazole | HCID 57434506 | — |
| 反応物 | HCID 58951512 | HCID 58951512 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | HCID 58951514 | HCID 58951514 | — |
反応手順
200 mg of tert-butyl 2-((1R,3S)-3-hydroxycyclohexylmethoxy)-2-methylpropionate are added dropwise as solution in MTBE to a suspension of 65 mg of sodium hydride (60% by weight in mineral oil) in 10 ml of MTBE. After gas evolution ceases, 503 mg of 4-iodomethyl-5-ethyl-2-(3-methoxyphenyl)oxazole are added as solution in MTBE, and the suspension is heated under reflux overnight. Ethyl acetate (MTBE can also be used) is added to the reaction mixture, and the mixture is washed with water and saturated sodium chloride solution, dried over magnesium sulfate and concentrated. The residue is chromatographed on silica gel (heptane/ethyl acetate gradient), resulting in 323 mg of tert-butyl 2-{(1R,3S)-3-[5-ethyl-2-(3-methoxyphenyl)oxazol-4-ylmethoxy]cyclohexylmethoxy}-2-methylpropionate as yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07956077B2 |
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| 出典データセット | uspto-grants-2011_06 |
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| ORD ID | ord-62b22e9b7ce2458c89cbbbb149e84a96 |
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| 出典メモ | uspto-grants-2011_06 |
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