関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Cyanocyclohexane | HCID 69834 | — |
| 反応物 | Ethane, 2-bromo-1,1-diethoxy- | HCID 74852 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 1-(2,2-Diethoxyethyl)cyclohexane-1-carbonitrile | HCID 13217350 | — |
反応手順
51.7 ml (0.5 mol) of anhydrous diethylamine are added dropwise to 312.5 ml (0.5 mol) of a 15% solution of n-butyl-lithium in hexane at -10° C. under an inert gas blanket. The batch is stirred for 10 minutes and then cooled to -70° C. Within 30 minutes, 54.6 g of cyclohexane-carbonitrile are added dropwise, after a further 30 minutes 98.5 g of bromoacetaldehyde-diethylacetal are added within 1 hour, and the batch is maintained for 24 hours at low temperature. Subsequently, it is warmed to room temperature, given onto 100 g of ice, extracted twice with 500 ml of ethyl acetate, the organic phase is dried over sodium sulfate, concentrated in vacuo, and the residue is subjected to vacuum distillation.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04515960 |
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| 出典データセット | uspto-grants-1985_05 |
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| ORD ID | ord-26fc452980d64f33bffc69f7d14a2f3a |
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| 出典メモ | uspto-grants-1985_05 |
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