関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 1-(Allyloxy)-5-methylhexane | HCID 86642018 | — |
| 触媒 | HCID 178527705 | HCID 178527705 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[(5-Methylhexyl)oxy]butanal | HCID 86642016 | 62% |
| 生成物 | 2-Methyl-3-[(5-methylhexyl)oxy]propanal | HCID 86642017 | 6.2% |
反応手順
Acetylacetanatodicarbonyl rhodium (I) (0.005 g, 0.02 mmol) and (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.030 g, 0.05 mmol) were added to a 25 mL glass-lined autoclave and dissolved in toluene (3 mL). 1-(allyloxy)-5-methylhexane (2.0 g, 12.2 mmol) was added to the reactor and, following purging with nitrogen, the reaction mixture was subjected to hydroformylation conditions using a 1:1 molar ratio of hydrogen and carbon monoxide gas (30 bar, 60° C., 4 h) with vigorous stirring. The reaction mixture was directly chromatographed on silica gel (hexane/diethyl ether). The isolated products were Kugelrolhr distilled to give 4-[(5-methylhexyl)oxy]butanal (1.4 g, 7.5 mmol, chemical yield 62%) and 2-methyl-3[(5-methylhexyl)oxy]propanal (0.14 g, 6.2%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088725B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-393579a63a764fc5ac75f66ce2ced8c1 |
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| 出典メモ | uspto-grants-2012_01 |
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