関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilyl triflate | HCID 65367 | — |
| 反応物 | 2,2,7,7-Tetramethyl-3,6-dioxa-2,7-disilaoctane | HCID 81858 | — |
| 反応物 | Methyl 3-oxocyclohexane-1-carboxylate | HCID 566099 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate | HCID 372311 | — |
反応手順
To a solution of trimethylsilyltrifluoromethanesulfonate (0.034 mL) in dry dichloromethane (5 mL) was added 1,2-bis(trimethylsiloxy)ethane (4.55 mL) followed by methyl 3-oxocyclohexanecarboxylate (2.9 g). The reaction mixture was stirred for 3 hours at −78° C. The reaction mixture was quenched with dry pyridine (0.5 mL), poured into saturated aqueous NaHCO3, and extracted with ether. The ether layer was dried over Na2CO3/Na2SO4. The reaction mixture was concentrated and purified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08580794B2 |
|---|
| 出典データセット | uspto-grants-2013_11 |
|---|
| ORD ID | ord-9050507d09314ffca3406ac1c87e0adb |
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| 出典メモ | uspto-grants-2013_11 |
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