関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethoxymethane | HCID 10024 | — |
| 反応物 | 1,1,2,3,3-Pentamethyl-hexahydro-4-indanol | HCID 21087577 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(Ethoxymethoxy)-1,1,2,3,3-pentamethyloctahydro-1H-indene | HCID 21087578 | 68.1% |
反応手順
A reaction flask was charged with 300 g (1.4 mole) 1,1,2,3,3-pentamethyl-hexahydro-4-indanol, 258 g (2.5 mole) diethoxymethane, 0.25 liter toluene, and 5 g boron trifluoride etherate complex. The reaction mass was heated to 100° C. and methanol and lite organics were collected in a Dean Stark trap (190 g recovered). After aging the reaction for 2 hrs the reaction was cooled to 25° C. and acid catalyst was quenched with 100 g of 10% aqueous sodium carbonate. The mass was transferred to a separatory funnel and water washed. The organic layer was separated and purified by fractional distillation. The procedure afforded a 68% yield (256 g) of 1,1,2,3,3-pentamethyl-octahydro-4-(ethoxymethoxy)-1H-indene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176324B1 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-5c1f3ef50c8146ed8cad4d29d17191f0 |
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| 出典メモ | uspto-grants-2007_02 |
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