関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoic Acid | HCID 243 | — |
| 反応物 | Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester | HCID 70670 | — |
| 反応物 | (1-Ethoxycyclopropoxy)trimethylsilane | HCID 2734686 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl cyclopropylideneacetate | HCID 11040705 | — |
反応手順
A suspension of 38.49 g (220.80 mmol) of [(1-ethoxycyclopropyl)oxy](trimethyl)silane, 100.0 g (287.04 mmol) of ethyl (triphenylphosphoranylidene)acetate and 3.51 g (28.70 mmol) of benzoic acid in 600 ml of toluene is stirred at a bath temperature of 90° C. for 18 hours. After cooling, the mixture is poured onto 800 g of silica gel 60 and eluted successively with in each case 3 liters of petroleum ether 40-60 and dichloromethane. The dichloromethane eluate is, after removal of the solvent, distilled at 160° C. and 14 mbar in a kugelrohr. This gives 17.95 g (64% of theory) of the title compound as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08168821B2 |
|---|
| 出典データセット | uspto-grants-2012_05 |
|---|
| ORD ID | ord-649bd9cf2f494c0480d63d8fb0fe56c5 |
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| 出典メモ | uspto-grants-2012_05 |
|---|
