関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclohexene | HCID 8079 | — |
| 反応物 | (3R)-1,1,3-trimethyl-2,3-dihydro-1H-inden-4-amine | HCID 14535936 | — |
| 触媒 | HCID 178418390 | HCID 178418390 | — |
| 生成物 | 1,1,3-Trimethylindan-4-amine | HCID 11217541 | — |
反応手順
Into a reaction vessel were charged 6.00 parts by weight of (3R)-1,1,3-trimethyl-4-aminoindane (optical purity of 96.5% ee) and 1.60 parts by weight of 5% palladium-carbon (STD-type, manufactured by N. E. Chemcat Corporation), thereby obtaining a mixture. The reaction vessel was sealed, the gas in the reaction vessel was replaced with nitrogen, and then the mixture was stirred at 150° C. to obtain a reaction mixture. While stirring the obtained reaction mixture, 1.40 parts by weight of cyclohexene was added dropwise thereto over 5 hours. Thereafter, the reaction mixture was cooled and filtered. The obtained solid was washed with 20 parts by weight of 2-propanol. The washing liquid recovered after washing and the filtrate obtained by filtration were combined. The combined mixture was concentrated under reduced pressure to obtain 5.63 parts by weight of 1,1,3-trimethyl-4-aminoindane. The obtained 1,1,3-trimethyl-4-aminoindane had an optical purity of 0.29% ee and a recovery rate of 93.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09284260B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-3c5b0c32142745efb9b0e9524251feb9 |
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| 出典メモ | uspto-grants-2016_03 |
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